Water → ethyl (Z)-2-ethoxy-3-(4-{6-[methyl-(4-nitrophenoxycarbonyl)amino]pyrid-2-yl}phenyl)acrylate

HRID 390588노트

반응식

HRID 390588 반응식
Cl[C:2]([O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1)=[O:3].C(N(C(C)C)CC)(C)C.[CH2:23]([O:25]/[C:26](=[CH:32]\[C:33]1[CH:38]=[CH:37][C:36]([C:39]2[CH:44]=[CH:43][CH:42]=[C:41]([NH:45][CH3:46])[N:40]=2)=[CH:35][CH:34]=1)/[C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH3:24].O>ClCCl>[CH2:23]([O:25]/[C:26](=[CH:32]\[C:33]1[CH:38]=[CH:37][C:36]([C:39]2[CH:44]=[CH:43][CH:42]=[C:41]([N:45]([CH3:46])[C:2]([O:4][C:5]3[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=3)=[O:3])[N:40]=2)=[CH:35][CH:34]=1)/[C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH3:24]

참가 물질

6

반응물 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 821294-Nitrophenyl chloroformateHCID 86626072ethyl (Z)-2-ethoxy-3-[4-(6-methylaminopyrid-2-yl)phenyl]acrylate

생성물 1

HCID 86626074ethyl (Z)-2-ethoxy-3-(4-{6-[methyl-(4-nitrophenoxycarbonyl)amino]pyrid-2-yl}phenyl)acrylate수율 110.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

0.55 g (2.75 mmol) of 4-nitrophenyl chloroformate and then 0.48 mL (2.75 mmol) of diisopropylethylamine are added to a solution of 0.6 g (1.84 mmol) of ethyl (Z)-2-ethoxy-3-[4-(6-methylaminopyrid-2-yl)phenyl]acrylate in 15 mL of dichloromethane. The reaction mixture is stirred for 1 hour 30 minutes at room temperature. The reaction is worked up by addition of 10 mL of water and extraction with dichloromethane. The organic phases are combined and then dried over magnesium sulfate, filtered and the solvent is evaporated off. 1 g (100%) of ethyl (Z)-2-ethoxy-3-(4-{6-[methyl-(4-nitrophenoxycarbonyl)amino]pyrid-2-yl}phenyl)acrylate is obtained in the form of a yellow oil.

후처리

  1. dry with materialdried over magnesium sulfate
  2. filtrationfiltered
  3. customthe solvent is evaporated off

출처 및 근거

ORD 기록
ord-5f85bd31d6b34cd89c7066ee24110862
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08383652B2

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