HRID476362
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 15 °C
PROCEDURE
实验过程
A mixture of N-[4-(4-amino-2,5-difluoro-phenoxy)-6-chloro-pyrimidin-2-yl]-acetamide (3.3 g, 10.5 mmol) and palladium on carbon (1.0 g, 10%) in methanol (100 mL) was stirred under H2 (1 atm) at 15° C. for 4 h. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure to give N-[4-(4-amino-2,5-difluoro-phenoxy)-pyrimidin-2-yl]-acetamide (2.4 g, 82% yield) as a pale yellow solid. 1HNMR (400 MHz, DMSO-d6): δ10.37 (s, 1H), 8.44 (d, J=5.7 Hz, 1H), 7.15 (dd, J=11.4 Hz, J=4.8 Hz, 1H) 6.71 (d, J=5.7 Hz, 1H), 6.65 (dd. J=12.3 Hz, J=8.4 Hz, 1H), 5.40 (s, 2H), 1.99 (s, 3H); MS (ESI) m/z: 281.2[M+H]+.
WORKUP
后处理
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate was concentrated under reduced pressure