반응식
[CH2:1]([O:3][C:4]([C:6]1[S:10][C:9]([NH:11][C:12]2[CH:17]=[C:16]([CH:18](OC)[O:19]C)[CH:15]=[CH:14][C:13]=2[N+:23]([O-:25])=[O:24])=[N:8][C:7]=1[C:26]1[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[CH:27]=1)=[O:5])[CH3:2].Cl>C(#N)C>[CH2:1]([O:3][C:4]([C:6]1[S:10][C:9]([NH:11][C:12]2[CH:17]=[C:16]([CH:18]=[O:19])[CH:15]=[CH:14][C:13]=2[N+:23]([O-:25])=[O:24])=[N:8][C:7]=1[C:26]1[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[CH:27]=1)=[O:5])[CH3:2]참가 물질
4
실험 절차
A mixture of 3.4 g (0.71 mmole) of 4-(3-chloro-phenyl)-2-(5-dimethoxymethyl-2-nitro-phenylamino)-thiazole-5-carboxylic acid ethyl ester (VI.41a), 80 mL of acetonitrile and 20 mL of 1M hydrochloric acid was heated 60 degrees for 30 minutes. The mixture was concentrated under reduced pressure, 200 mL of water was added and the pH was adjusted to 9 by the addition of 15% sodium hydroxide solution. The precipitate was collected by filtration to give 3.0 g of 4-(3-chloro-phenyl)-2-(5-formyl-2-nitro-phenylamino)-thiazole-5-carboxylic acid ethyl ester (VI.41b) as a white solid.
후처리
- temperaturewas heated 60 degrees for 30 minutes
- concentrationThe mixture was concentrated under reduced pressure, 200 mL of water
- additionwas added
- additionthe pH was adjusted to 9 by the addition of 15% sodium hydroxide solution
- filtrationThe precipitate was collected by filtration
출처 및 근거
- ORD 기록
- ord-868149746958472ba167f992e660b573
- 출처 데이터셋
- uspto-grants-2011_10
- 특허 번호
- US08044213B2
연결된 노트
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