반응식
C(N(CC)C(C)C)(C)C.Cl[C:11]1[C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:15][N:14]=[C:13]([S:22][CH3:23])[N:12]=1.Cl.[Cl:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[NH:32][NH2:33]>O1CCCC1>[Cl:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[NH:32][NH:33][C:11]1[C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:15][N:14]=[C:13]([S:22][CH3:23])[N:12]=1참가 물질
5
실험 절차
At room temperature, 16.2 mL of N,N-diisopropylethylamine was added to tetrahydrofuran (300 mL) solution of 9.4 g of ethyl 4-chloro-2-(methylthio)pyrimidine-5-carboxylate and 8.3 g of 2-chlorophenylhydrazine hydrochloride, and heated under reflux for 18 hours. The solvent was concentrated under reduced pressure, water was added to this, and extracted with ethyl acetate, and the ethyl acetate layer was washed with saturated saline water, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure to obtain crude ethyl 4-[2-(2-chlorophenyl)hydrazino]-2-(methylthio)pyrimidine-5-carboxylate as a yellow oily substance.
후처리
- temperatureheated
- temperatureunder reflux for 18 hours
- concentrationThe solvent was concentrated under reduced pressure, water
- additionwas added to this, and
- extractionextracted with ethyl acetate
- washthe ethyl acetate layer was washed with saturated saline water
- dry with materialdried with anhydrous sodium sulfate
- customThe solvent was evaporated away under reduced pressure
출처 및 근거
- ORD 기록
- ord-48d5b8a2b45f43f19f7c8741247eb5ef
- 출처 데이터셋
- uspto-grants-2011_05
- 특허 번호
- US07935708B2
연결된 노트
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