Category: iodides-buliding-blocks

116632-41-8, name is 2-Chloro-5-iodotoluene, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. SDS of cas: 116632-41-8

To a mixture of 2-chloro-5-iodotoluene (4.07 g, 16.12 mmol), iV-bromosuccinimide (3.16 g, 17.73 mmol) in dichloromethane (258 mL) and water (258 mL) was added 2,2′- azodiisobutyronitrile (0.132 g, 0.81 mmol). The reaction mixture was irradiated with a halogen sun lamp (150 watt) for 2 h and then cooled to room temperature. The two-phase reaction mixture was separated, and the aqueous layer was extracted with dichloromethane (50 mL). The combined organic layers were washed with water (2 x 150 mL), dried over magnesium sulfate, filtered and concentrated under reduced pressure to provide the title compound as an orange oil (5.20 g).1H NMR (CDCl3): 57.76 (d, 1H), 7.58 (d, 1H), 7.11 (d, 1H), 4.49 (s, 2H).

The synthetic route of 116632-41-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; WO2008/124092; (2008); A2;,
Iodide – Wikipedia,
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Synthetic Route of 3210-08-0,Some common heterocyclic compound, 3210-08-0, name is 4-Iodobutan-1-ol, molecular formula is C4H9IO, 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.

N,N?-dibutylpiperazine (50.4 mmol, 10 g) and 4-iodobutanol (40.3 mmol, 8.1 g) were used in the same manner as Example 1, except that reaction was carried out at room temperature for 10 hours. In this manner, a compound represented by [Chemical Formula 5] was obtained (yield 85.6%). (0062) 1H NMR (300 MHz, DMSO) delta=0.89-0.91 (m, 6H), 1.29-1.52 (m, 8H), 1.71 (m, 4H), 2.80 (t, 6H), 3.01 (t, 2H), 3.22 (t, 4H), 3.34 (t, 4H), 3.46 (t, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Iodobutan-1-ol, its application will become more common.

Reference:
Patent; KOREA INSTITUTE OF SCIENCE AND TECHNOLOGY; LEE, Hyun Joo; LEE, Ung; KIM, Hong Gon; CHO, Shinhye; LEE, He Won; (16 pag.)US2020/155997; (2020); A1;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 3718-88-5, name is 3-Iodobenzylamine hydrochloride, molecular formula is C7H9ClIN, 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. Safety of 3-Iodobenzylamine hydrochloride

To 36 B-1 (0.30 g, 1.0 mmol), 818 3-iodobenzylamine hydrochloride (0.33 mg, 1.2 mmol), 14triethylamine (0.43 mL, 3.1 mmol), 169 WSC hydrochloride (0.29 g, 1.5 mmol) and 637 1-hydroxy-7-azabenzotriazole (69 mg, 0.51 mmol) was added 12 dichloromethane (10 mL), and the mixture was stirredat room temperature for 24 hr. To the reaction mixture was added 52 water, and the mixture was extractedwith dichloromethane. The organic layer was dried over sodium sulfate. The desiccant was filtered off, andthe solvent was evaporated. The obtained residue was purified by high performance liquid chromatography(water-acetonitrile, each containing 0.1% 80 trifluoroacetic acid) to give the 819 title compound (0.29 g , 0.56 mmol, 55%). MS (ESI) m/z 511 (M+H)+

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3718-88-5, its application will become more common.

Reference:
Patent; EA PHARMA CO., LTD.; KOBAYASHI, Kaori; SUZUKI, Tamotsu; KAWAHIRA, Mizuki; FUJII, Tomohiro; SUGIKI, Masayuki; OHSUMI, Koji; OKUZUMI, Tatsuya; (285 pag.)US2016/332999; (2016); A1;,
Iodide – Wikipedia,
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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., SDS of cas: 34270-90-1

A stirred solution of Intermediate 71 (0.8 g, 2.42 mmol) and 1-iodo-2-(2-iodoethoxy)ethane (0.38 mL, 2.67 mmol) in anhydrous DMF (16 mL) was cooled to -l5C30 and purged with nitrogen for 5 minutes, then caesium carbonate (3.16 g, 9.69 mmol) wasadded. The reaction mixture was stirred for 2 h, with warming to 20C. Water (30 mL)was added and the aqueous layer was extracted with tert-buty1 methyl ether (3 x 30 mL).The combined organic layers were washed with water (2 x 30 mL) and brine (30 mL), then dried over sodium sulfate, filtered and concentrated. The resulting crude materialwas purified by flash column chromatography, using a gradient of tert-buty1 methyl etherin heptane (0-15%), to afford the title compound (927.9 mg, 86%) as a yellow solid. DH(500 MHz, CDCb) 7.90 (d, J 1.3 Hz, 1H), 7.06 (dd, J9.1, 1.6 Hz, 1H), 4.26 (t, J 11.8 Hz,5 2H), 3.89 (dd, J 11.9, 3.6 Hz, 2H), 2.45-2.33 (m, 2H), 1.75-1.69 (m, 2H), 1.65 (s, 9H).HPLC-MS (method 5): [M+H-BOC]+ m/z 300.0, 302.0, RT 2.11 minutes.

According to the analysis of related databases, 34270-90-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UCB BIOPHARMA SPRL; BRACE, Gareth Neil; CHAPPELL, Rose Elizabeth; DEBOVES, Herve Jean Claude; FOLEY, Anne Marie; FOULKES, Gregory; JONES, Elizabeth Pearl; LECOMTE, Fabien Claude; QUINCEY, Joanna Rachel; SCHULZE, Monika-Sarah Elisabeth Dorothea; SELBY, Matthew Duncan; SMALLEY, Adam Peter; TAYLOR, Richard David; TOWNSEND, Robert James; ZHU, Zhaoning; (278 pag.)WO2018/229079; (2018); A1;,
Iodide – Wikipedia,
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Application of 608-28-6, These common heterocyclic compound, 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, 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.

Add 0.2 mmol of potassium carbonate,0.005 mmol of tris (dibenzylideneacetone) dipalladium,1,3-bis (diphenylphosphine) propane 0.02mmol,18-crown-6-ether 0.1mmol,1,3-dimethyl-2-iodobenzene 0.1 mmol,1-phenyl-1-hexyne 0.25 mmol and1 mL of N, N-dimethylformamide was added to a 15 mL reaction tube,Fill with nitrogen repeatedly 10 times, stir at room temperature for 15 min, add 0.5 mmol of water, and place in a reaction dish at 100 C for 16 h; cool to room temperature, dilute the reaction solution with ethyl acetate, wash with water, and dry the organic phase with anhydrous Na2SO4 , Filtered, concentrated, and purified by thin layer chromatography to obtain 14.9 mg of the target product as a colorless oil with a yield of 57%.

Statistics shows that 2-Iodo-1,3-dimethylbenzene is playing an increasingly important role. we look forward to future research findings about 608-28-6.

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (12 pag.)CN110256184; (2019); A;,
Iodide – Wikipedia,
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Related Products of 124700-41-0,Some common heterocyclic compound, 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid, molecular formula is C7H4FIO2, 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 1 (20.0 g, 75.2 mmol, 1 eq) was dissolved in 70 mL of EtOH.Then gradually add H2SO4 (7.37g, 75.1mmol, 4.01mL, 1eq).The mixture was stirred at 100 C for 5 h.And use TLC (Dichloromethane/Methanol=10/1, Rf=0.87) The progress of the reaction was detected.When the reaction is complete,The reactants were concentrated under reduced pressure.The concentrated product was extracted (EOtOH 200 mL, NaHCO 3 saturated solution (100.0 mL x 2), and then the organic layer was taken.It was dried by adding anhydrous Na2SO4.After further evaporation to dryness the title product 2 (21.0 g, 71.4 mmol, 94.9% yield).Figure 3 shows the results of TLC chromatography for this reaction.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Fluoro-5-iodobenzoic acid, its application will become more common.

Reference:
Patent; Shanghai Health Medical School; Tang Dewei; Huang Gang; Huang Chen; Wu Xingyu; Yu Meicen; Li Yanjiao; (18 pag.)CN109942582; (2019); A;,
Iodide – Wikipedia,
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Reference of 3210-08-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 3210-08-0, name is 4-Iodobutan-1-ol belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Method B: Compound 3(68.9 mg, 0.074 mmol) was allowed to stir overnight in THF(10 mL) at 55 C. The solvent was removed from the product toafford pure 4 as a pale orange solid (65 mg, 87% yield). Yellow crystalssuitable for X-ray crystallography were grown from a concentratedCH2Cl2 solution of compound 4. 1H NMR (400 MHz, CD2Cl2):d 7.74 (m, 4H, Ar-H), 7.59 (m, 2H, Ar-H), 7.46 (m, 2H, Ar-H), 7.41(m, 8H, Ar-H), 7.27 (m, 2H, Ar-H), 7.18 (m, 2H, Ar-H), 7.07 (m,8H, Ar-H), 4.01 (m, 2H, O-CH2CH2CH2CH2-I), 3.88 (br, 2H, CH2),2.96 (m, 2H, O-CH2CH2CH2CH2-I), 2.54 (br, 2H, CH2), 1.67 (m, 2H,O-CH2CH2CH2CH2-I), 1.39 (m, 2H, O-CH2CH2CH2CH2-I). 31P NMR(161.8 MHz, CD2Cl2): d 93.1 (br, 1P), 10.7 (br, 2P). 13C NMR(100.5 MHz, C6D6): d 147.0, 135.6, 135.3, 134.1, 131.5, 130.0,129.6, 128.6, 124.3, 123.5, 66.8, 47.6, 33.2, 30.3, 7.0. Anal. Calc.for C42H40N2OP3CuI2: C, 50.49; H, 4.04; N, 2.80. Found: C, 50.22;H, 3.99; N, 2.77%.

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-Iodobutan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Knight, Sadie E.; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Inorganica Chimica Acta; vol. 422; (2014); p. 181 – 187;,
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. 13421-13-1, name is 4-Chloro-2-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 13421-13-1

General procedure: To an oven dried three neck RB containing 2-Iodobenzoic acid (1) (2mmol), benzyl amine (2) (4mmol) and CuI(0.4mmol) in DMSO(3ml) was added 0.55g of K2CO3. Then, the reaction mixture was allowed to stir at 90C under air atmosphere for 12h.The completion of the reaction was monitored by TLC. After being cooled at room temperature the reaction mixture was poured in to ice cooled water and extracted with ethyl acetate two times. The combined organic layer was washed with brine and then dried over anhydrous Na2SO4. The solvent was evaporated and the crude product was purified by column chromatography (hexane(80)/ ethyl acetate (20)) on silica gel to afford 2-phenyl-4H-benzo[d][1,3]oxazine-4-one.

According to the analysis of related databases, 13421-13-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Munusamy, Sathishkumar; Venkatesan, Sathesh; Sathiyanarayanan, Kulathu Iyer; Tetrahedron Letters; vol. 56; 1; (2015); p. 203 – 205;,
Iodide – Wikipedia,
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In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 628-21-7, name is 1,4-Diiodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 628-21-7

Preparation 122 4′-Chlorospiro[cyclopentane-1,5′-pyrrolo[2,3-d]pyrimidin]-6′(7’H)-one Add 4-chloro-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one (0.6 g; 0.0035 mol; 1.0 equiv) in anhydrous THF (20 mL) and cool the reaction to -78 C., under an inert atmosphere. Add drop-wise lithium hexamethyldisilazide (8.8 mL; 0.0088 mol; 2.5 equiv; 1M in THF). Stir at -78 C. for 30 min. Add drop-wise 1,4-diiodobutane (0.56 mL; 0.0042 mol; 1.2 equiv), allow the reaction temperature to reach 0 C. slowly, and stir for 2 h. Then allow the reaction to reach RT and stir for additional 1 h. Quench the reaction with saturated ammonium chloride solution and extract with EA. Wash the organic layer with water, brine, and dry over anhydrous sodium sulfate. Evaporate the organic layer and purify over a 10 g silica column with acetone (5%) in DCM. Pool fractions to give the title compound (0.34 g; 43.09%). H NMR (DMSO-d6):11.68 (1H, s), 8.53 (1H, s), 2.0-2.1 (m, 2H), 1.91-1.99 (m, 6H).

The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shepherd, Timothy Alan; Dally, Robert Dean; Joseph, Sajan; US2010/120801; (2010); A1;,
Iodide – Wikipedia,
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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. 19099-54-8, name is 1-Iodo-2-isopropylbenzene, A new synthetic method of this compound is introduced below., Quality Control of 1-Iodo-2-isopropylbenzene

General procedure: To a mixture of the catalyst 3 (20mg containing 0.05mol% Pd for aryl iodides and 40mg containing 0.1mol% Pd for aryl bromides and chlorides), aryl halide (1mmol), alkyne (1.5mmol), and K2CO3 (1.5mmol, 207mg) was added PEG 200 (2mL) under argon atmosphere. The reaction mixture was stirred for the appropriate reaction time at 85 or 130C (see, Table 2). The progress of the reaction was monitored by using gas chromatography. After completion of the reaction, pure products were obtained by using column chromatography with hexane and ethyl acetate as eluents.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Gholinejad, Mohammad; Dasvarz, Neda; Najera, Carmen; Inorganica Chimica Acta; vol. 483; (2018); p. 262 – 270;,
Iodide – Wikipedia,
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