N-[4-({[tert-butyl(dimethyl)silyl]oxy}methyl)-2-chloro-5-methoxyphenyl]-acrylamide → HCID 178493273, 화합물

HRID 630386노트

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HRID 630386 반응식
[Si:1]([O:8][CH2:9][C:10]1[C:15]([O:16][CH3:17])=[CH:14][C:13]([NH:18][C:19](=[O:22])[CH:20]=[CH2:21])=[C:12]([Cl:23])[CH:11]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[OH:24][C:25]([C:42]1[S:43][CH:44]=[CH:45][CH:46]=1)([C:37]1[S:38][CH:39]=[CH:40][CH:41]=1)[C:26]([O:28][C@H:29]1[CH2:34][CH2:33][C@H:32]([NH:35][CH3:36])[CH2:31][CH2:30]1)=[O:27]>C(Cl)Cl>[OH:24][C:25]([C:37]1[S:38][CH:39]=[CH:40][CH:41]=1)([C:42]1[S:43][CH:44]=[CH:45][CH:46]=1)[C:26]([O:28][C@H:29]1[CH2:30][CH2:31][C@H:32]([N:35]([CH2:21][CH2:20][C:19]([NH:18][C:13]2[CH:14]=[C:15]([O:16][CH3:17])[C:10]([CH2:9][O:8][Si:1]([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2])=[CH:11][C:12]=2[Cl:23])=[O:22])[CH3:36])[CH2:33][CH2:34]1)=[O:27]

참가 물질

4

반응물 2

HCID 67145019N-[4-({[tert-butyl(dimethyl)silyl]oxy}methyl)-2-chloro-5-methoxyphenyl]-acrylamide2회HCID 178484861HCID 178484861, 화합물2회

생성물 1

HCID 178493273HCID 178493273, 화합물수율 49%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
75 °C

실험 절차

A mixture of N-[4-({[tert-butyl(dimethyl)silyl]oxy}methyl)-2-chloro-5-methoxyphenyl]-acrylamide (intermediate 40; 0.9 g, 0.002 mol) and trans-4-(methylamino)cyclohexyl hydroxy(di-2-thienyl)acetate (intermediate 5; 0.7 g, 0.002 mol) in methylene chloride (20 mL) was stirred at 75° C. in a closed vessel for 64 hours. The solvent was evaporated and the crude obtained was purified by column chromatography with silica gel, eluting with chloroform/methanol (from 50/1 to 25/1) to give the title compound as a white-yellow solid (49%).

후처리

  1. customThe solvent was evaporated
  2. customthe crude obtained
  3. customwas purified by column chromatography with silica gel
  4. washeluting with chloroform/methanol (from 50/1 to 25/1)

출처 및 근거

ORD 기록
ord-fb23a10b75c84c1896e13a76cba18296
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315463B2

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