Formamidine acetate → 4-(Dimethoxymethyl)pyrimidine
반응식
[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]=1참가 물질
4
반응 조건
- 온도
- 120 °C
실험 절차
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]+.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-3901f8e046ba4e618c832ed2155d01c4
- 출처 데이터셋
- uspto-grants-2015_07
- 특허 번호
- US09073908B2
반응 노트
불러오는 중…