Tag: M.W=300-400

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 6326-42-7, name is Methyl 2-iodo-4-nitrobenzoate, 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 6326-42-7, SDS of cas: 6326-42-7

[0001173] To a mixture of ammonium chloride (122 g) and iron (38.2 g) in ethanol (1000 mL) and water (100 mL) was added Example 2.140.2 (70 g,) at room temperature. The mixture was stirred at 80 C for 4 hours and filtered to remove insoluble material. The filtrate was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (1000 mL) and washed with water (500 mL). The aqueous phase was extracted with ethyl acetate (1000 mL x 2). The combined organic phase was washed with brine, dried over MgSO/i, filtered and concentrated to give the title compound. MS (LC-MS) m/e 278.0 (M+H)+.

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, Methyl 2-iodo-4-nitrobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ABBVIE INC.; TAO, Zhi-Fu; DOHERTY, George; WANG, Xilu; SULLIVAN, Gerard M.; SONG, Xiaohong; KUNZER, Aaron R.; WENDT, Michael D.; MARIN, Violeta L.; FREY, Robin R.; CULLEN, Steve C.; WELCH, Dennie S.; SHEN, Xiaoqiang; BENNETT, Nathan B.; HAIGHT, Anthony R.; ACKLER, Scott L.; BOGHAERT, Erwin R.; SOUERS, Andrew J.; JUDD, Andrew S.; (623 pag.)WO2016/94509; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 672-57-1, The chemical industry reduces the impact on the environment during synthesis 672-57-1, name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

4-Chloro-3-iodobenzenetrifluoride (306 mg) was dissolved in toluene (3 ml), and thereto were added 2-ethynylpyridine (155 mg), copper iodide (19.0 mg), 1,3-bis-(2,6-diisopropylphenyl)-imidazolium chloride (42.5 mg), acetic acid palladium (II) (22.5 mg) and cesium carbonate (489 mg), and the mixture was heated to 100 C. After the mixture was stirred for 3 h, the mixture was kept standing to cool to room temperature, and thereto were added 3-amino-6-methoxypyridine (149 mg) and potassium-t-butoxide (168 mg), and the reaction mixture was heated to 100 C. After the reaction mixture was stirred all day and all night, it was kept standing to cool to room temperature, and to the reaction solution were added ethyl acetate and water. After an insoluble material was filtrated, the organic layer was separated. The organic layer was washed with a saturated saline and dried with anhydrous sodium sulfate. After the organic layer was filtrated and concentrated, the residue was purified by the silica gel column chromatography affording the compound 2 (77.0 mg).MS m/z 370 [M+H]+, APCI(+)

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, 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Mitsubishi Tanage Pharma Corporation; US2012/258951; (2012); A1;,
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. 628-77-3, name is 1,5-Diiodopentane, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C5H10I2

A solution of Compound 33 (50.0 mg, 0.20 mmol) in DMF (5.0 mL) was added K2CO3 (42.26 mg, 0.31 mmol) and 1,5-diiodopentane (333 mg, 1.0 mmol). The reaction mixture was stirred at 90 C. for 3 h. The reaction mixture was purified by silica chromatography (0-50% EtOAC in petroleum ether) to give (S)-8-((5-hydroxypentyl)oxy)-7-methoxy-1,2,3,11a-tetrahydro-5H-benzo[e]pyrrolo[1,2-a]azepin-5-one 34 (60 mg, 0.178 mmol, 87.6% yield) as an oil. LCMS (5-95AB/1.5 min): RT=0.765 min, [M+H]+ 332.0

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 628-77-3.

Reference:
Patent; Genentech, Inc.; Dragovich, Peter; Pillow, Thomas; Sadowsky, Jack; Sliwkowski, Mark X.; Wei, BinQing; (160 pag.)US2017/95570; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 173406-17-2 as follows. Recommanded Product: 173406-17-2

To a mixture of 244 mg of 3- (2-aminoetliyl) pyridine (2.0 mmol) and 604 mg of t-butyl 3- iodobenzoate (2.0 mmol) in 10 [ML] of toluene was added 250 mg of sodium t-butoxid (2.5 [MMOL),] 30 mg [OF TRI-T-BUTYLPHOSPLIONIMN TETAFLUOROBORATE] (0.1 mmol) and 50 mg of tris (dibenzylidineacetone) dipalladium [(0)] (0.055 [MMOL).] The mixture was stirred for 16 h and filtered through celite. The celite was washed with 3 X 5 mL of toluene and the filtrate was concentrated in vacuo. The residue was purified by column [CHROMATOGRAPHY] using 35%-45% EtOAc in hexanes as eluant to give 103 mg of t-butyl N- (2- (3-pyridyl) ethyl)-3-aminobenzoate as a bright yellow oil (17% yield).

According to the analysis of related databases, 173406-17-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MEMORY PHARMACEUTICALS CORPORATION; WO2004/9552; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 450412-29-0, A common heterocyclic compound, 450412-29-0, name is 1-Bromo-3-fluoro-2-iodobenzene, molecular formula is C6H3BrFI, 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.

28.3 g (100 mmol, 1.0 eq.) m-bromoiodobenzene and 25.8 g m-bromoaniline (150 mmol, 1.5 eq.)It was placed in a dry 3 L three-necked flask, and then dried and degassed 1100 ml of toluene was added as a solvent.Nitrogen gas was passed for 15 minutes. Add 2.9g (15% mol) of cuprous iodide,5.9 g (30% mol) of 1,10-phenanthroline and 63.7 g (300 mol, 3 eq.) potassium phosphate.The temperature was raised to 110 C and the reaction was carried out for 18 hours. After the reaction is completed, cool to room temperature, suction filtration,Rotating to remove the solvent,Recrystallization with toluene and ethanol,27.8 g of intermediate L were obtained,The yield was 85%.

The synthetic route of 450412-29-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nanjing Gao Guang Semiconductor Materials Co., Ltd.; Jin Zhenyu; Qian Chao; Wang Xiaowei; Dai Peipei; (49 pag.)CN108164511; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 148836-41-3,Some common heterocyclic compound, 148836-41-3, name is 1-Bromo-4-chloro-2-iodobenzene, molecular formula is C6H3BrClI, 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.

General procedure: An oven-dried Schlenk tube was charged with a magneticstir bar, binucleophile 2-mercaptobenzimidazole 2 (1.0 mmol, 1.0 equiv), CuI(0.1 mmol, 10 mol %), phen (0.2 mmol, 20 mol %), and K2CO3 (2.0 mmol, 2equiv). The tube was capped and then evacuated and backfilled with nitrogen(3 times). Under a positive pressure of nitrogen, a solution of o-dihaloarene 1(1.05 mmol, 1.05 equiv) in DMF (3 mL) was added via syringe. The tube wassealed and allowed to stir at 120 C (monitored by TLC). After being cooled toroom temperature, EtOAc (40 mL) was added and the mixture was washedwith brine (20 mL 3). The organic phase was dried over Na2SO4 andconcentrated. The residue was purified by column chromatography on silicagel using petrol/EtOAc (10:1?3:1, v:v) as eluent to give product 3.

The synthetic route of 148836-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gao, Jilong; Zhu, Jiaoyan; Chen, Lubin; Shao, Yingying; Zhu, Jiaqi; Huang, Yijia; Wang, Xiaoxia; Lv, Xin; Tetrahedron Letters; vol. 55; 22; (2014); p. 3367 – 3373;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 25252-00-0,Some common heterocyclic compound, 25252-00-0, name is 2-Bromo-5-iodobenzoic acid, molecular formula is C7H4BrIO2, 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.

Oxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo-5-iodo-benzoic acid (49.5 g) in CH2CI2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h. Then, the solution is concentrated under reduced pressure and the residue is dissolved in THF (100 mL). The resulting solution is cooled in an ice-bath and L1BH4 (3.4 g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2S04) and the solvent is evaporated under reduced pressure to give the crude product. Yield: 47.0 g (99% of theory)

The synthetic route of 25252-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM VETMEDICA GMBH; KLEY, Saskia; REICHE, Dania Birte; WO2015/110402; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 21740-00-1, name is 5-Bromo-2-iodobenzoic 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 21740-00-1, Recommanded Product: 5-Bromo-2-iodobenzoic acid

5-Bromo-2-iodobenzoic acid (409 mg, 1.25 mmol), A7-(3-dimethylaminopropyl)-iV- ethylcarbodiimide hydrochloride (288 mg, 1.5 mmol ), 1 -hydroxy benzotriazole (135 mg, 1.0 mmol), AVV-diisopropylethylamine (523 pL, 3.0 mmol), and benzylamine (109 pL, 1.0 mmol) were dissolved in anhydrous DMF (5 mL) and stirred at room temperature for 16 hr. The reaction mixture was diluted with an excess of EtOAc and washed five times with water and brine. The organic layer was dried over NarSOy filtered and concentrated. The residue was purified by flash column chromatography (EtOAc : DCM = 0 : 100 to 30 : 70) to give A-benzyl- 5-bromo-2~iodobenzamide (361 mg, 87 %) as a white solid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Bromo-2-iodobenzoic acid, and friends who are interested can also refer to it.

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.)WO2019/164949; (2019); A1;,
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. 628-77-3, name is 1,5-Diiodopentane, This compound has unique chemical properties. The synthetic route is as follows., category: iodides-buliding-blocks

Spiro[cyclohexane-1,3′-[3H]indol]-2′-(1’H)one A solution of oxindole (25 g, 0.19 mol) in anhydrous tetrahydrofuran (800 cm3) was cooled to -20 C., then n-butyllithium (2.5M in hexanes, 152 cm3, 0.38 mol) was added slowly followed by N,N,N’,N’-tetramethylethylenediamine (51 cm3, 0.38 mol,). After 15 min. 1,5-diiodopentane (174 g, 0.54 mol) was added slowly and the mixture was allowed to warm to room temperature. After stirring for 16 h. saturated aqueous ammonium chloride solution (1L) and EtOAc (1L) were added. After 15 min. the layers were separated and the aqueous phase was extracted EtOAc (*2). The combined organic layers were extracted with hydrochloric acid (1N), then washed with brine (500 cm3), dried (MgSO4), and concentrated to obtain an oil. The oil was triturated with hexane (200 cm3) and benzene (20 cm3). The precipitate was collected and dried in vacuo to obtain the title compound (26.3 g, 69.6%) as colorless crystals: mp 110-114 C.; 1H NMR (DMSO-d6) delta 1.67 (m, 10H), 6.84 (d, 1H, J=8 Hz) 6.94 (t, 1H, J=8 Hz), 7.17 (t, 1H, J=8 Hz), 7.44 (d, 1H, J=8 Hz), 10.3 (S, 1H).

According to the analysis of related databases, 628-77-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Wyeth; Ligand Pharmaceuticals, Inc.; US6462032; (2002); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com