Phosphorus oxychloride → 2-(3-((2-Amino-4-chloro-6-methylpyrimidin-5-yl)methyl)-4-methoxyphenyl)acetonitrile
반응식
[NH2:1][C:2]1[N:7]=[C:6](O)[C:5]([CH2:9][C:10]2[CH:11]=[C:12]([CH2:18][C:19]#[N:20])[CH:13]=[CH:14][C:15]=2[O:16][CH3:17])=[C:4]([CH3:21])[N:3]=1.O=P(Cl)(Cl)[Cl:24]>>[NH2:1][C:2]1[N:7]=[C:6]([Cl:24])[C:5]([CH2:9][C:10]2[CH:11]=[C:12]([CH2:18][C:19]#[N:20])[CH:13]=[CH:14][C:15]=2[O:16][CH3:17])=[C:4]([CH3:21])[N:3]=1참가 물질
3
반응 조건
- 온도
- 90 °C
실험 절차
The product from step (ii) (2.8 g) was added to POCl3 (25 ml) and heated at 90° C. for 15 h and then evaporated under reduced pressure. The residue was diluted with ice/water (20 mL) and the mixture adjusted to pH ˜7 with sodium bicarbonate. The mixture was heated at 50° C. for 1 h and the precipitate collected by filtration. The solid was dried under vacuum to give the subtitle compound as a brown solid, 2.88 g.
후처리
- customevaporated under reduced pressure