Water → HCID 86585161、化合物
反応式
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]=1参加物
6
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-a18ccc6edf4f4b28822d832105a9ff5f
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07449472B2
反応ノート
読み込み中…