Water → HCID 86585161, 화합물
반응식
Cl[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[S:9])=[CH:6][N:5]=[C:4]([CH3:13])[N:3]=1.[CH3:14][NH2:15].O>ClCCl.C(O)C>[CH3:14][NH:15][C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[S:9])=[CH:6][N:5]=[C:4]([CH3:13])[N:3]=1참가 물질
6
실험 절차
To a 0° C. solution of 20 g (86 mmol) of ethyl 4-chloro-2-methylthiopyrimidine-5-carboxylate (Aldrich Chemical Co., Milwaukee, Wis., USA) in 250 mL of dichloromethane was slowly added 35 mL (281 mmol) of a 33% solution of methylamine in ethanol. After stirring for 30 minutes, 150 mL of water was added and the phases were separated. The organic phase was dried over magnesium sulfate and filtered. The filtrate was evaporated under reduced pressure to give 19 g (97%) of ethyl 4-methylamino-2-methylthiopyrimidine-5-carboxylate as a white solid.
후처리
- customTo a 0° C.
- customthe phases were separated
- dry with materialThe organic phase was dried over magnesium sulfate
- filtrationfiltered
- customThe filtrate was evaporated under reduced pressure
출처 및 근거
- ORD 기록
- ord-a18ccc6edf4f4b28822d832105a9ff5f
- 출처 데이터셋
- uspto-grants-2008_11
- 특허 번호
- US07449472B2
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