Aniline → methyl 3-anilino-2-(3,4-dimethylbenzoyl)prop-2-enoate

HRID 226920

반응식

HRID 226920 반응식
[CH3:1][O:2][C:3](=[O:18])[C:4]([C:8](=[O:17])[C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[C:11]([CH3:16])[CH:10]=1)=[CH:5]OC.[NH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>>[CH3:1][O:2][C:3](=[O:18])[C:4]([C:8](=[O:17])[C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[C:11]([CH3:16])[CH:10]=1)=[CH:5][NH:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

참가 물질

3

반응물 2

HCID 6115AnilineHCID 668792722-(3,4-Dimethyl-benzoyl)-3-methoxy-acrylic acid methyl ester

생성물 1

HCID 178500752methyl 3-anilino-2-(3,4-dimethylbenzoyl)prop-2-enoate수율 46.6%

실험 절차

Crude 2-(3,4-dimethyl-benzoyl)-3-methoxy-acrylic acid methyl ester 1a(13.7 g, 55.1 mmol) and of aniline (5.12 g, 55.1 mmol) were heated neat at 100° C. for 30 minutes, then cooled down to room temperature and recrystallized from dichloromethane/hexane to yield 7.94 g of 2-(3,4-Dimethyl-benzoyl)-3-phenylamino-acrylic acid methyl ester 2a as a yellow crystalline solid: LC-MSD, m/z for C19H19NO3 [M+H]+=310.4; HPLC retention time: 2.8 min.

후처리

  1. customrecrystallized from dichloromethane/hexane

출처 및 근거

ORD 기록
ord-02efdeed9b914c61b224ccc77a38b1ad
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07557213B2

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