Month: July 2021

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 6828-35-9, name is 5-Chloro-2-iodoaniline, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 5-Chloro-2-iodoaniline

Under nitrogen protection, 4-((1S,4S)-4-(but-3-yn-2-yl)cyclohexyl)-6-fluoroquinoline (110 mg,0.39 mmol), 5-chloro-2-iodoaniline (99 mg, 0.39 mmol) and Et3N (118 mg, 1.2 mmol) of N,N-dimethylacetamideCuI (8 mg, 0.04 mmol) and Pd(PPh3)2Cl2 (29 mg, 0.04 mmol) were sequentially added to the solution (3 mL), and the reaction mixture was added.The reaction was stirred at room temperature for 4 h. TLC showed that after the reaction of the starting material was completed, NaOH (160 mg, 4.0 mmol) was added, and the temperature was raised to 140.Stir at C overnight, cool to room temperature, add water to the reaction mixture to quench, extract three times with EA, and combine with organicWash with brine, dry with anhydrous Na2SO4,The crude product obtained by concentration is passed through a thin layer chromatography plate.(DCM / MeOH = 25 / 1) was isolated and purified to give the title compound (90 mg, yield: 77%) as pale yellow solid.

According to the analysis of related databases, 6828-35-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Chengdu Hai Borui Pharmaceutical Co., Ltd.; Chengdu Beite Pharmaceutical Co., Ltd.; Huang Haoxi; Liu Guanfeng; Ren Junfeng; Yi Shoubing; Chen Tonghun; He Quanhong; Wu Xiancai; Li Yingfu; Su Zhonghai; (97 pag.)CN109574988; (2019); A;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 35453-19-1, Safety of 5-Amino-2,4,6-triiodoisophthalic acid

Preparation (A); Synthesis of 5-Amino-2,4,6-triiodo-isophthaloyl dichloride (1); 5-Amino-2,4,6-triiodo-isophtalic acid (30 g, 0.054 mol) (commercially available from Aldrich), thionyl chloride (8.2 ml, 0.113 mol) and pyridine (0.2 ml) in 1,2 dichloroethane (20 ml) were heated to 70 0C. A portion of thionyl chloride (15.2 ml, 0.21 mol) was added dropwise during VA o 2 hrs, and the mixture was heated to 85 0C for 6 hrs. After cooling the reaction mixture to room temperature, it was poured into 30Og of ice-water. The yellow precipitate that formed was filtered off, sucked dry and then washed with water until washings showed a pH of ca 5. The filter cake was then dried in a vacuum oven at 500C for 3 hrs. A light yellow powder was obtained 31 g (~ quant.) as the desired product.13C NMR (DMSOcZ6) 66, 78.4, 148.9, 149.2, 169MS (ES-) found 593.5 [M-H+], expected 593.7; Example 8; N,N’,N”-Tris-[(3(N-2,3-dihydroxypropylcarbamoyl)-2,4,6-triiodo-1-hydroxyl acetamide) phenyl] carbamoyl methyl ethane; Starting material and all other materials were commercially available from Aldrich. a) 5-amino-2,4,6-triiodo-isophtaloyl chloride; 5-Amino-2,4,6-triiodo-isophtalic acid (30 g, 0.054 mol), thionyl chloride (8.2 ml, 0.113 mol) and pyridine (0.2 ml) in 1,2 dichloroethane (20 ml) were heated to 70 0C. A portion of thionyl chloride (15.2 ml, 0.21 mol) was added dropwise during VA to 2 hrs, and the mixture was heated to 85 0C for 6 hrs. After cooling the reaction mixture to room temperature, it was poured into 30Og of ice-water. The yellow precipitate that formed was filtered off, sucked dry and then washed with water until washings showed a pH of ca 5. The filter cake was then dried in a vacuum oven at 50C for 3 hrs. A light yellow powder was obtained 31 g (~ quant.) as the desired product.13C NMR (DMSOd6) 66, 78.4, 148.9, 149.2, 169MS (ES-) found 593.5 [M-H+], expected 593.7FT-IR (cm”1) 3471, 3372 (NH), 1777 (C=O).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; GE HEALTHCARE AS; WO2007/94683; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 460-37-7, A common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Compound 2 was added to 21 three-necked bottles(5 (^, 0.167111 O1), 0.5111 O1 / 1He 0 field of liquid(84011 ^), stirmixLOmin. A solution of trifluoroiodopropaneLt; / RTI & gt;The reaction was stirred at room temperature4-5 hours.Add 5001 ^AcetateThe organic phase was dried over anhydrous sodium sulfate, filtered and the filtrate was evaporated to dryness to give 55.5 g of a yellow solid in 84% yield.

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang Yongning Pharmaceutical Co., Ltd; YE, TIANJIAN; LU, XIUWEI; YU, GUAMGLIANG; HE, SI; PAN, PENG; TIAN, JIAHUA; (10 pag.)CN105949258; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 13194-68-8, name is 4-Iodo-2-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., name: 4-Iodo-2-methylaniline

(a) Preparation of 4-Fluoro-2-(4-iodo-2-methyl-phenylamino)-benzoic acid To a stirred solution containing 3.16 g (0.0133 mol) of 2-amino-5-iodotoluene in 5 mL of tetrahydrofuran at -78 C. was added 10 mL (0.020 mol) of a 2.0 M lithium diisopropylamide in tetrahydrofuran/heptane/ethylbenzene (Aldrich) solution. The resulting green suspension was stirred vigorously for 15 minutes, after which time a solution of 1.00 g (0.00632 mol) of 2,4-difluorobenzoic acid in 10 mL of tetrahydrofuran was added. The reaction 2,4-difluorobenzoic acid in 10 mL of tetrahydrofuran was added. The reaction temperature was allowed to increase slowly to room temperature, at which temperature the mixture was stirred for 2 days. The reaction mixture was concentrated by evaporation of the solvent under reduced pressure. Aqueous HCl (10%) was added to the concentrate, and the solution was extracted with dichloromethane. The organic phase was dried (MgSO4) and then concentrated over a steambath to low volume (10 mL) and cooled to room temperature. The off-white fibers which formed were collected by vacuum filtration, rinsed with hexane, and dried in a vacuum-oven (76 C.; ca. 10 mm of Hg) to afford 1.10 g (47%) of the desired material; mp 224-229.5 C.; 1H NMR (400 MHz, DMSO): delta9.72 (s, 1H), 7.97 (dd, 1H, J=7.0, 8.7 Hz), 7.70 (d, 1H, J=1.5 Hz), 7.57 (dd, 1H, J=8.4, 1.9 Hz), 7.17 (d, 1H, J=8.2 Hz), 6.61-6.53 (m, 2H), 2.18 (s, 3H); 13C NMR (100 MHz, DMSO): delta169.87, 166.36 (d, JC-F=249.4 Hz), 150.11 (d, JC-F=11.4 Hz), 139.83, 138.49, 136.07, 135.26 (d, JC-F=11.5 Hz), 135.07, 125.60, 109.32, 104.98 (d, JC-F=21.1 Hz), 99.54 (d, JC-F=26.0 Hz), 89.43, 17.52; 19F NMR (376 MHz, DMSO): delta-104.00 to -104.07 (m); IR (KBr) 1670 (C=O stretch)cm-1; MS (CI) M+1=372. Analysis calculated for C14H11FINO2: C, 45.31; H, 2.99; N, 3.77. Found: C, 45.21; H, 2.77; N, 3.64.

According to the analysis of related databases, 13194-68-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Barrett, Stephen Douglas; Bridges, Alexander James; Doherty, Annette Marian; Dudley, David Thomas; Saltiel, Alan Robert; Tecle, Haile; US2003/78428; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 2043-55-2, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 2043-55-2 as follows.

Into a pressure resistant autoclave (0.5 liter) equipped with stirring vanes (disk turbine), FI, potassium (meth)acrylate, PTZ and BuOH were charged in the amounts (unit: mol) as shown in Table 1, and an ester-forming reaction was carried out under the reaction conditions shown in Table 1 to obtain a reaction mixture. The conversion and selectivity of the reaction are shown in Table 1.

According to the analysis of related databases, 2043-55-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Asahi Glass Company, Limited; EP1486482; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 34270-90-1, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane, This compound has unique chemical properties. The synthetic route is as follows.

Cesium carbonate (20.7 g, 63.5 mmol) was added portionwise over a 20 minute period to a stirred solution of tert-butyl 6-bromo-2-oxoindoline-1-carboxylate (preparation 8a, 6.0 g, 16.0 mmol) and 1-iodo-2-(2-iodoethoxy)ethane (6.58 g, 17.6 mmol) in N,N’-dimethylformamide (250 mL) at -20 C under an argon atmosphere. After the addition the mixture was warmed to room temperature and stirred for 3 hours. Acetic acid (1.1 mL) followed by ethyl acetate and water were added to the reaction mixture and the organic layer was separated, washed with water, dried (MgSO4) and evaporated. Purification of the residue by flash chromatography (10:1 to 5:1 hexanes/ethyl acetate) gave the title compound (4.50 g, 61%) as a pale yellow solid. LRMS (m/z): 382/384 (M+1)+. 1H-NMR delta (CDCl3): 1.65 (s, 9H), 1.86 (m, 4H), 3.90 (m, 2H), 4.23 (m, 2H), 7.17(d, J=7.97 Hz, 1H), 7.33 (d, J=7.97 Hz, 1H), 8.07 (s, 1H)

The chemical industry reduces the impact on the environment during synthesis 1-Iodo-2-(2-iodoethoxy)ethane. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Laboratorios Almirall, S.A.; EP2108641; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 61272-76-2, The chemical industry reduces the impact on the environment during synthesis 61272-76-2, name is 4-Fluoro-2-iodoaniline, I believe this compound will play a more active role in future production and life.

A’-Benzyl~2~iodo~5~meihoxybenzamide (1.61 g, 4.38 mmol), 4-fIuoror-2-iodoani.ine (867 mg, 3.66 mmol), copper (I) iodide (139 mg, 0.73 mmol), and potassium carbonate (1.26 g, 9.12 mmol) were taken up in anhydrous DMSG (24 mL) and the resulting reaction mixture and the resulting reaction mixture was first stirred at 80 C for 2 hours, followed by heating to 135 C for another 16 hours. After cooling to room temperature, the mixture was filtered over celite and concentrated. The residue was diluted with an excess of Et?0 and washed with water. The organic layer was dried over Na2S04, filtered and concentrated. The residue was purified by flash column chromatography (EtOAc : Hex = 0: 100 to 100:0; then EtOAc : DCM = 0: 100 to 25:75) to give 10-Benzyl-8-fluoro-2-methoxy-5,lO-dihydro-l IH- dibenzo[6,e][1,4]diazepin~ i l~one (565 mg, 44%) as a light yellow foam.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-Fluoro-2-iodoaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DANA-FARBER CANCER INSTITUTE, INC.; GRAY, Nathanael S.; DE CLERCQ, Dries; JANG, Jaebong; JANNE, Pasi; TO, Ciric; ECK, Michael; PARK, Eunyoung; HEPPNER, David; (0 pag.)WO2019/164941; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 6828-35-9, name is 5-Chloro-2-iodoaniline, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 6828-35-9, SDS of cas: 6828-35-9

General procedure: Aryl iodide or bromides (5.0 mmol),paraformaldehyde (5.0 mmol), Pd(OAc)2 (0.0005 mmol) (for aryliodides) or Pd(PPh3)4 (0.05 mmol) (for aryl bromides) andCs2CO3 (7.0 mmol) were reacted in DMSO at 80 oCfor 12 h. The reaction mixture was poured into H2O, and extractedwith Et2O. The internal standard (dodecane) was added to theresulting mixture, and the conversion of aryl iodide and the yield of thehydrodehalogenated product were calculated.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 5-Chloro-2-iodoaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Pyo, Ayoung; Kim, Sudeok; Kumar, Manian Rajesh; Byeun, Aleum; Eom, Min Sik; Han, Min Su; Lee, Sunwoo; Tetrahedron Letters; vol. 54; 38; (2013); p. 5207 – 5210;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 5460-32-2, name is 4-Iodo-1,2-dimethoxybenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 4-Iodo-1,2-dimethoxybenzene

General procedure: The appropriate 2-amino-5H-benzothiopyrano[4,3-d]pyrimidine 22a-c (0.417mmol) was added, at room temperature, under nitrogen atmosphere, to 0.079g of CuI (0.417mmol) and 0.115g of anhydrous K2CO3 (0.833mmol). Then, the appropriate substituted aryl iodide (0.694mmol), 0.04mL of DMEDA (0.417mmol) and 2.5mL of dioxane were added. The reaction mixture was heated at 100°C and allowed to stir for 24h. After cooling, the reaction mixture was added with 2.5mL of concentrated NH3 and with a saturated solution of NaCl (10-15mL). The mixture was extracted with ethyl acetate. The organic phase was dried (MgSO4) and evaporated under reduced pressure giving a residue which was purified by flash chromatography using petroleum ether 60-80°C/ethyl acetate 5:5 as the eluting system, to give compounds 1-21. 4.1.1.16 2-(3,4-Dimethoxyanilino)-5H-benzothiopyrano[4,3-d]pyrimidine (16) Yield: 40percent; m. p. 148-149?°C; 1H NMR (400?MHz, DMSO-d6): delta 3.72 (s, 3H), 3.78 (s, 3H), 4.01 (s, 2H), 6.91 (d, J?=?8.8?Hz, 1H), 7.26 (dd, Jmin?=?2.2?Hz, Jmax?=?8.6?Hz, 1H), 7.36-7.43 (m, 3H), 7.63 (d, J?=?1.2?Hz, 1H), 8.31 (d, J?=?7.6?Hz, 1H), 8.44 (s, 1H), 9.51 (s, 1H) ppm; 13C NMR (100?MHz, DMSO-d6): delta 25.94, 55.29, 55.87, 104.27, 110.54, 112.37, 114.59, 126.12, 126.95, 127.93, 131.14, 132.22, 134.34, 136.56, 143.61, 148.53, 156.54, 157.55, 159.42?ppm; HRMS (ESI) m/z calculated for C19H18N3O2S ([M+H]+) 352.11197, found 352.11067. Anal. C19H17N3O2S (C, H, N).

The synthetic route of 5460-32-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Salerno, Silvia; Garcia-Argaez, Aida Nelly; Barresi, Elisabetta; Taliani, Sabrina; Simorini, Francesca; La Motta, Concettina; Amendola, Giorgio; Tomassi, Stefano; Cosconati, Sandro; Novellino, Ettore; Da Settimo, Federico; Marini, Anna Maria; Via, Lisa Dalla; European Journal of Medicinal Chemistry; vol. 150; (2018); p. 446 – 456;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 69113-59-3, The chemical industry reduces the impact on the environment during synthesis 69113-59-3, name is 3-Iodobenzonitrile, I believe this compound will play a more active role in future production and life.

General Procedure (Stille Coupling). A mixture of aryl iodide (1.00 equiv), organostannane (1.00 equiv) and cesium fluoride (3.00 equiv) in DMF was cooled to 0 C. and degassed for 10 mm with argon. Then Pd(PPh3)4 (0.10 equiv) and Cul (1.20 equiv) were added to the mixture and the reaction mixture was stirred for 0.5 h at 60 C. under argon. Afier the reaction was complete, the reaction mixture was diluted with CH2C12 and water, shaken vigorously and filtered through celite with ethyl acetate. The organic layer was separated, washed with brine, dried over anhydrous Na2504, and concentrated. The product was purified by colunm chromatography on silica gel using ethyl acetatehexanes. The general Stille coupling procedure was followed using 3-iodobenzonitrile 40 (35 mg, 0.15 mmol), organostannane 54 (120 mg, 0.184 mmol), CsF (69 mg, 0.46 mmol), Pd(PPh3)4 (17 mg, 0.015 mmol) and Cul (34 mg, 0.18 mmol) in dry DMF (8 mE). The reaction mixture was stirred for 21 h and the product was purified by column chromatography on silica gel using 15% ethyl acetate-hexanes to give the product 21(64 mg, 90%) as a oil: ?H NMR (270 MHz, CDC13) 0 7.54-7.41 (m, 4 H), 7.06 (s, 1 H), 7.00 (s, 1 H), 6.10 (t, J=7.4 Hz, 1 H), 4.10 (s, 3 H), 3.86 (s, 3 H), 2.82 (t, J=7.4 Hz, 2 H), 2.48 (s, 3 H), 2.33 (s, 3 H), 2.30-2.23 (m, 2 H), 1.95 (quint, J=7.4 Hz, 2 H); ?3C NMR (68 MHz, CDC13) 0 166.3, 163.5, 155.8, 143.0, 139.8, 134.3, 133.8, 133.7, 132.5, 131.2, 130.8, 130.6, 130.5,129.4, 128.9, 127.2, 118.7, 112.3, 63.0, 61.3, 29.1, 26.4,24.8, 16.4, 11.0; ElMS mlz (rd intensity) 464 (M, 2.0), 466 (M+2, 0.7), 398 (17), 397 (51), 299 (13), 98 (100); HRMS (El) for C25H2535C1N403 calcd 464.1615 (Mj, found 464. 1600, C25H2537C1N403 calcd 466.1586 (M+2), found 466.1584.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-Iodobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Purdue Research Foundation; Cushman, Mark S.; Sakamoto, Takeshi; (32 pag.)US2017/267667; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com