HRID1159877
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
- 80 °C
PROCEDURE
实验过程
To a solution of N-(2,3-dihydro-1,4-benzodioxin-6-yl)-4-[2-(3-nitrophenyl)pyrazolo[1,5-a]pyridin-3-yl]-2-pyrimidinamine (1.09 g, 2.3 mmol) in ethanol (2 mL) was added sodium sulfide nonhydrate (2.76 g, 11.5 mmol) in H2O (2 mL). The mixture was heated at 80° C. for 16 h, allowed to cool to rt and filtered. The filtrate was concentrated to afford the product (1 g) as a yellow solid. 1H NMR (400 MHz, d6-DMSO) 69.29 (s, 1H), 8.76 (d, 1H, J=7.2), 8.51 (d, 1H, J=8.8), 8.15 (d, 1H, J=5.2), 7.39-7.43 (m, 1H), 7.35 (m, 1H), 7.04-7.12 (m, 3H), 6.76-6.72 (m, 2H), 6.65-6.62 (m, 2H), 6.43 (d, 1H, J=5.2), 5.21 (s, 2H), 4.16-4.20 (m, 4H).
WORKUP
后处理
- temperatureto cool to rt
- filtrationfiltered
- concentrationThe filtrate was concentrated