Category: chlorides-buliding-blocks

Related Products of 432-21-3,Some common heterocyclic compound, 432-21-3, name is 2-Amino-6-chlorobenzotrifluoride, molecular formula is C7H5ClF3N, 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.

[00221] A mixture of 49.3 (50 mg, 0.134 mmol), 3-chloro-2-(trifluoromethyl)aniline (40 mg, 0.2 mmol) and aqueous Na2C03 solution (2 N, 0.80 mmol) in i-PrOH/H20 (10:1 , 4 ml_) was degassed with N2. Then Pd(PPh3)2CI2 (10 mg, 0.0134 mmol) was added to. The reaction suspension was degassed with N2 and heated at 100 C for 30 min by microwave reactor. The reaction mixture was diluted with EA and washed with water. The combined organic layers was dried over anhydrous Na2S04 and filtered. The filtrate was evaporated to give the crude which was purified by prep-HPLC (0.1 % TFA/ACN/ H20) to give the title compound (4.6 mg, 5%). 1H NMR (300 MHz, DMSO-cf6) delta ppm 7.76 (d, 2H), 7.63 – 7.53 (m, 4H), 7.31 (t, 1 H), 7.17 (dd, 2H), 6.93 (d, 1 H), 6.62 (d, 1 H), 3.85 (s, 3H), 3.63 (s, 2H). LC-MS: [M+H]+ = 407.8.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Amino-6-chlorobenzotrifluoride, its application will become more common.

Reference:
Patent; NOVARTIS AG; HE, Feng; DU-CUNY, Lei; XIAO, Qitao; XUN, Guoliang; ZHENG, Qiangang; (152 pag.)WO2017/149463; (2017); A1;,
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Synthetic Route of 883499-24-9,Some common heterocyclic compound, 883499-24-9, name is 1-Bromo-2-chloro-3-fluorobenzene, molecular formula is C6H3BrClF, 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.

In a nitrogen atmosphere, a flask containing 114 7-(diphenylamino)-9,9?-dimethyl-9H-fluoren-3-ol (100 g), 123 1-bromo-2-chloro-3-fluorobenzene (58.3 g), 77 potassium carbonate (91.5 g), and NMP (500 ml) was heated and stirred at a reflux temperature for four hours. After the reaction was stopped, the reaction liquid was cooled to room temperature, and 30 water was added thereto. A precipitate thus precipitated was collected by suction filtration. The obtained precipitate was washed with water and then with methanol and then purified by silica gel column chromatography (eluent: toluene) to obtain an intermediate 124 6-(3-bromo-2-chlorophenoxy)-9,9-dimethyl-N,N-diphenyl-9H-fluoren-2-amine (150 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2-chloro-3-fluorobenzene, its application will become more common.

Reference:
Patent; JNC CORPORATION; FUJITA, Yukihiro; (228 pag.)US2019/165279; (2019); A1;,
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Adding a certain compound to certain chemical reactions, such as: 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, belongs to chlorides-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 2533-69-9, COA of Formula: C3H4Cl3NO

To a solution of 2,3-diamino-benzamide (302 mg, 2 mmol) in ether (12 mL) and DCM(9mL), methyl 2,2,2-trichloroacetimidate (0.44 mL, 2.5 mmol) and TFA (1.0 mL, 12.8 mmol)were added. The reaction mixture was stirred at room temperature for 6 h. After evaporation, andchromatography (DCM/methanol=70:1) gave the title compound 5 as a white solid (340 mg,61.3%).

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 2,2,2-trichloroacetimidate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zhou, Jie; Ji, Ming; Zhu, Zhixiang; Cao, Ran; Chen, Xiaoguang; Xu, Bailing; European Journal of Medicinal Chemistry; vol. 132; (2017); p. 26 – 41;,
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Application of 261762-56-5, These common heterocyclic compound, 261762-56-5, name is 1-Chloro-2-fluoro-3-methoxybenzene, 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.

2-Chloro-3-fluoro-4-methoxybenzaldehyde 1g (6.2 mmol) 3-Chloro-2-fluoroanisole in 20 ml THF was cooled to -70C and 2.7 ml of a 2.5 M n-butyl lithium solution in hexane were added. After one hour at -70 3.93 ml DMF in 7 ml THF were added at -70C and the mixture is stirred another hour at -70C. 15 ml of a 1 M aqueous hydrochloric acid were added and the reaction was warmed to ambient temperature over 18 hours. The reaction mixture was partitioned between diethyl ether and water. The aqueous phase was extracted with diethyl ether, the combined organic phases were washed with brine, dried over sodium sulfate and evaporated. The crude product was purified by chromatography on silica gel to yield 0.25 g 2-chloro-3-fluoro-4-methoxybenzaldehyde. 1H-NMR (CDCl3); delta = 3.98 (s, 3H), 6.98 (dd, 1H), 7.75 (dd, 1H), 10.30 (s, 1H).

The synthetic route of 261762-56-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bayer Schering Pharma Aktiengesellschaft; AstraZeneca AB; EP2149558; (2010); A1;,
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461432-23-5, name is 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene, belongs to chlorides-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: 461432-23-5

To a solution of Example IB (200 g, 0.614 mol) in anhydrous toluene/TEtaF (1.2 L, 2:1 (v/v)) was added n-BuLi (2.5 M in hexane, 295 mL) dropwise at -65 0C. The reaction was stirred at -65 0C for 30 min. Then the mixture was transferred by a cannula to a solution of (5i?,^5i?,(5i?)-3,4,5-tris(trimethylsilyloxy)-6-((trimethylsilyloxy)methyl)tetrahydro-2/f- pyran-2-one) (373 g, 0.798 mol) in toluene (1.2 L ) at -65 0C. The mixture was stirred at -65 0C until starting material was consumed (2 h). The reaction was quenched with hydrochloric acid (36-38%, 113 mL, 1.35 mol) in methanol (800 mL), and stirred at room temperature overnight. The reaction was neutralized with saturated sodium bicarbonate to pEta 7.5 and the organic phase was separated and the aqueous phase was extracted with ethyl acetate (2 x 3.0 L). The combined organic layers were washed with brine (2 x 2.0 L), dried over sodium sulfate and concentrated. The residue was dissolved in hot toluene (600 mL) and poured into n-hexane (2.0 L) with vigorous stirring. After stirring for Ih, the mixture was filtered and the filter cake was dried under vacuum to give the desired product as a white solid. This solid was used without further purification in the next step. MS ESI (m/z) 439[M+1]+

The synthetic route of 461432-23-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THERACOS, INC.; LIOU, Jason; WU, Yuelin; LI, Shengbin; XU, Ge; WO2010/22313; (2010); A2;,
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These common heterocyclic compound, 933190-51-3, name is 8-Bromo-6-chloroimidazo[1,2-b]pyridazine, 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. Safety of 8-Bromo-6-chloroimidazo[1,2-b]pyridazine

A mixture of 8-bromo-6-chloroimidazo[l,2-b]pyridazine (573 mg, 2.47 mmol), 6-(3-tert- butylpyrrolidin-l-yl)pyridin-2-amine (540 mg, 2.47 mmol), Pd2(dba)3 (142 mg, 0.25 mmol), BINAP (307 mg, 0.50 mmol), Cs2C03 (2.4 g, 7.41 mmol) and dioxane (20 mL) was heated to reflux with stirring for 15 h under N2. The solvent was removed in vacuo and the resulting mixture was purified by chromatography (silica gel, 200 – 300 mesh, dichloromethane : MeOH = 50 : 1) to give N-(6-(3-tert-butylpyrrolidin-l-yl)pyridin-2-yl)-6-chloroimidazo [l,2-b]pyridazin- 8-amine (400 mg, crude) as a brown oil. LC-MS: [M+H]+, 371.1 , tR = 2.23 min.

The synthetic route of 8-Bromo-6-chloroimidazo[1,2-b]pyridazine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HERMANN, Johannes Cornelius; KUGLSTATTER, Andreas; LUCAS, Matthew C.; PADILLA, Fernando; WANNER, Jutta; ZHANG, Xiaohu; WO2013/64445; (2013); A1;,
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Some common heterocyclic compound, 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, molecular formula is C4H6Cl2, 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. COA of Formula: C4H6Cl2

To a solution of 0.235 g of (+)-(1-Benzyloxycarbamoyl-but-3-enyl)-carbamic acid tert-butyl ester (9a) in 8 mL of tetrahydrofuran was added 0.635 g of cesium carbonate. The reaction was heated to 60oC for 60 minutes, and then 1 mL of 2-chloro-3-methallyl chloride was added. The reaction was heated for an additional 20 hours. The reaction was then cooled, quenched with NH4Cl(aq.) solution, and extracted with ethyl acetate. The organic layers were washed with NH4Cl(aq.) and NaCl(aq.) solutions. The aqueous layers were re-extratced with ethyl acetate, and the organic layers combined and dried over Na2SO4(s). Filtration and solvent removal gave a white, oily solid. Column chromatography (hexanes/ethyl acetate gadiant) on silica gel, followed by fraction combination, and solvent removal gave 170 mg of a white solid (57% yield). 1H NMR (CDCl3): d 2.36 (quint, 1H, J=7 Hz), 2.48 (quint, 1H, J=7 Hz), 4.06 (d, 2H, J=4 Hz), 4.12 (m, 1H), 4.68 (m, 1H), 4.88 (bs, 1H), 4.99 (m, 2H), 5.13 (m, 1H), 5.26 (m, 2H), 5.72 (m, 1H), 7.4 (m, 5H); MS: 839 (2M+Na), 431 (M+Na).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1871-57-4, its application will become more common.

Reference:
Article; Wilson, Lawrence J.; Wang, Bingbing; Yang, Shyh-Ming; Scannevin, Robert H.; Burke, Sharon L.; Karnachi, Prabha; Rhodes, Kenneth J.; Murray, William V.; Bioorganic and Medicinal Chemistry Letters; vol. 21; 21; (2011); p. 6485 – 6490;,
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Some common heterocyclic compound, 928782-97-2, name is 4-Chloro-2-(phenylethynyl)aniline, molecular formula is C14H10ClN, 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. name: 4-Chloro-2-(phenylethynyl)aniline

General procedure: The substituted 2-alkynylaniline (1.0 mmol) was dissolved in acetonitrile (5.0 mL) and stirred until the solution became homogeneous. To this solution, methyl vinyl ketone (1.5 mmol) followed by 20 mol % of PdCl2 (59-60%, 35 mg) was added under a nitrogen atmosphere, then heated to 60 C and monitored by TLC. After completion of the reaction, the mixture was cooled to room temperature and the acetonitrile was removed by vacuum evaporation. The resulting crude product was purified by column chromatography to afford the desired 2,3-disubstituted indoles. 1-(5-Chloro-2-phenyl-1H-indol-3-yl)pentan-3-one (3n) Yield: (300 mg, 96%); Colorless solid. Mp: 138-140 C. FT-IR (KBr) (nu/cm-1): 3370, 1711. 1H NMR (400 MHz, CDCl3) deltaH (ppm): 8.10 (br s, 1H), 7.55-7.53 (m, 3H), 7.47 (t, J=7.5 Hz, 2H), 7.40-7.36 (m, 1H), 7.27 (d, J=8.56 Hz, 1H), 7.15 (dd, J=8.5, 1.9 Hz, 1H), 3.15-3.11 (m, 2H), 2.77-2.73 (m, 2H), 2.39 (q, J=7.3 Hz, 2H), 1.03 (t, J=7.3 Hz, 3H). 13C NMR (100 MHz, CDCl3) deltaC (ppm): 211.1, 136.1, 134.4, 132.7, 130.1, 129.2, 128.3, 128.1, 125.5, 122.7, 118.6, 112.1, 111.9, 43.1, 36.2, 18.9, 7.9. LRMS (EI) (m/z) (relative intensity): 311 (M+, 50), 328 (100); HRMS calcd for C19H18Cl1O1N1 (M+): 311.1077, found 311.1086.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 928782-97-2, its application will become more common.

Reference:
Article; Janreddy, Donala; Kavala, Veerababurao; Kuo, Chun-Wei; Kuo, Ting-Shen; He, Chiu-Hui; Yao, Ching-Fa; Tetrahedron; vol. 69; 15; (2013); p. 3323 – 3330;,
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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. 7051-16-3, name is 1-Chloro-3,5-dimethoxybenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: chlorides-buliding-blocks

3-Chloro-5-methoxy-phenol3-Chloro-5-methoxy-phenolSodium methanelhiolate (3.04 g, 43.37 mmol), was added to a solution of l-chloro-3.5- dimethoxy benzene (5.0 g, 28.96 mmol) in 20 ml of l-Methyl-2-Pyrrolidone and the reaction mixture was heated at 140 C for 2.5 h then stirred at room temperature over night. l-Methyl-2-pyrrolidone was removed under reduced pressure and the material partitioned between ethyl acetate/water/lN hydrochloric acid. The organic layer was washed twice with IN hydrochloric acid, brine, dried over sodium sulfate and solvent removed under reduced pressure to give a yellowish solid. The solid was purified by column chromatography (silica gel 60-120 mesh, 10:90 ethylacetate:hexane) to afford 3- Chloro-5-methoxy-phenol in 76.4 % yield.MS [M-H] 157.2, ? NMR (400 MHz, CDCI3) delta (ppm): 6.455-6.500 (d, 2H, J=I8.0 Hz), 6.291 (s, 1H), 4,978 (s, III), 3.767 (s, 3H).

The synthetic route of 7051-16-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JUBILANT BIOSYS LTD.; SARMA, Pakala Kumara Savithru; ACHARYA, Vinod Parameshwaran; KASIBHATLA, Srinivas Rao; VISWANADHAN, Vellarkad Narayana; TIWARI, Atul; SINGHA, Rakesh Kumar; BISCHOFF, Alexander; (149 pag.)WO2012/90219; (2012); A2;,
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Adding a certain compound to certain chemical reactions, such as: 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, belongs to chlorides-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 61881-19-4, Product Details of 61881-19-4

To 6 (5.0 g, 5 mmol) and N-phenyl trifluoroacetimidoyl chloride (1.6 g, 7.5 mmol, 1.5 eq) in acetone (103.0 ml) was added K2CO3 (1.0 g, 7.5 mmol, 1.5 eq). The mixture was stirred at room temperature for 1 h. The reaction was monitored by TLC (hexane : ethyl acetate = 2:1) .The mixture was filtered, concentrated, and purified by silica gel column chromatography (hexane : ethyl acetate = 4:1) to obtain the 9 (5.7 g, 96%) as white solid. m. p.132 – 134 oC. [alpha]25D = – 213.6 (c = 1.00 in CHCl3).1H NMR (400 MHz, CDCl3) delta 8.49 – 6.58 (m, 36H), 6.28 (d, J = 10.5 Hz, 1H), 6.01 (d, J = 3.2 Hz, 1H), 5.93 (dd, J = 10.5, 3.4 Hz, 1H), 5.76 (s, 1H), 5.65 (dd, J = 10.5, 3.1 Hz, 1H), 4.98 (d, J = 8.9 Hz, 1H), 4.55 – 4.34 (m, 4H), 4.17 (d, J = 12.0 Hz, 1H), 3.98 (dd, J = 13.1, 1.8 Hz, 1H), 3.92 (d, J = 9.6 Hz, 1H), 1.75 (s, 3H). 13C NMR (100 MHz, CDCl3) delta 170.1-164.83 (C, C=O), 143.2 (C, N-C), 141.0 (F3CC=N), 133.6-128.1 (C, Ar), 124.9, 119.2,116.2 (q, CF3), 106.3, 99.1, 70.2, 69.9, 69.7, 69.1, 68.5, 66.8, 63.9, 63.3, 61.9, 58.3, 20.3. ESI-MS (m/z) : [M+Na]+ : calcd for C62H52F3NO18Na+ 1202.3029, found 1202.3028.

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, 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zhang, Hongliang; Wang, Hengtao; Xu, Qiulong; Lu, Rui; Cao, Yunhua; Wang, Zhefeng; Tang, Pingping; Lin, Feng; Li, Yingxia; Carbohydrate Research; vol. 448; (2017); p. 6 – 9;,
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