Triethylamine → 3-(N-methyl-methoxycarbamoyl)-5-nitro benzoic acid allyl ester

HRID 1977352

반응식

HRID 1977352 반응식
[CH2:1]([O:4][C:5](=[O:25])[C:6]1[CH:7]=[C:8]([CH:19]=[C:20]([N+:22]([O-:24])=[O:23])[CH:21]=1)[C:9]([O:11]N1C(=O)CCC1=O)=O)[CH:2]=[CH2:3].Cl.[CH3:27][NH:28][O:29][CH3:30].C(N(CC)CC)C>ClCCl>[CH2:1]([O:4][C:5](=[O:25])[C:6]1[CH:21]=[C:20]([N+:22]([O-:24])=[O:23])[CH:19]=[C:8]([C:9](=[O:11])[N:28]([O:29][CH3:30])[CH3:27])[CH:7]=1)[CH:2]=[CH2:3]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 229860995-Nitro-isophthalic acid 1-(2,5-dioxo-pyrrolidin-1-yl) ester 3-allyl ester

생성물 1

HCID 206558613-(N-methyl-methoxycarbamoyl)-5-nitro benzoic acid allyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of (7(b)) (2.00 g), N,O-dimethylhydroxylamine hydrochloride (0.62 g), triethylamine (0.86 ml) and dichloromethane (60 ml) was stirred at 5° for 30 min and then allowed to warm to ambient temperature and stirred for a further 16 h. The mixture was poured onto a flash column and eluted with ethyl acetate/hexane (40:60)to give 3-(N-methyl-methoxycarbamoyl)-5-nitro benzoic acid allyl ester (7(c)) as a yellow oil.

후처리

  1. stirringstirred for a further 16 h
  2. additionThe mixture was poured onto a flash column
  3. washeluted with ethyl acetate/hexane (40:60)to

출처 및 근거

ORD 기록
ord-fa852f342c674df3a82b19d74e6f6a87
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06232338B1

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