Formamidine acetate → 4-(Dimethoxymethyl)pyrimidine
反応式
[CH3:1][N:2](C)/[CH:3]=[CH:4]/[C:5](=O)[CH:6]([O:9][CH3:10])[O:7][CH3:8].C(O)(=O)C.C(N)=[NH:18]>O>[CH3:8][O:7][CH:6]([O:9][CH3:10])[C:5]1[CH:4]=[CH:3][N:2]=[CH:1][N:18]=1参加物
4
反応条件
- 温度
- 120 °C
実験手順
A mixture of (E)-4-dimethylamino-1,1-dimethoxy-but-3-en-2-one (49.6 g, 286 mmol) and formamidine acetate (44.7 g, 429 mmol) was heated at 120° C. for 4 h. After cooling to room temperature the mixture was poured into water and extracted with dichloromethane. The combined organic extracts were then dried over sodium sulfate, filtered and evaporated. Purification by distillation afforded the title product (31 g, 70%) as a colourless liquid. Bp 59-60° C. at 1.3 mbar. MS: m/e=155.0 [M+H]+.
後処理
- temperatureAfter cooling to room temperature the mixture
- extractionextracted with dichloromethane
- dry with materialThe combined organic extracts were then dried over sodium sulfate
- filtrationfiltered
- customevaporated
- customPurification
- distillationby distillation
出典と根拠
- ORDレコード
- ord-3901f8e046ba4e618c832ed2155d01c4
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09073908B2
反応ノート
読み込み中…