HRID1694384
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
- 50 °C
PROCEDURE
实验过程
Methyl 4-{1-[({1-[4-(trifluoromethyl)benzyl]-1H-indol-7-yl}carbonyl)amino]cyclopropyl}benzoate (27 g, 55 mmol) was dissolved in 549 ml of THF 549 ml of MeOH and 249 ml of a 2M solution of KOH. The mixture was heated at 50° C. for 2 h. After cooling to RT, 200 ml of water was added and the organic solvents removed. The solution was acidified to pH 1-1.5 with 3N HCl and the resulting solid was filtered and washed with water. 1H NMR (500 MHz, DMSO-d6): δ 12.80 (bs, 1H), 9.15 (s, 1H), 7.80 (d, 3H), 7.60 (d, 2H), 7.50 (d, 1H), 7.40 (d, 1H), 7.25-7.11 (m, 3H), 6.90 (d, 2H), 6.65 (d, 1H), 5.70 (s, 2H), 1.15 (m, 2H), 0.90 (m, 2H). MS−ESI (477.4).
WORKUP
后处理
- temperatureAfter cooling to RT
- customthe organic solvents removed
- filtrationthe resulting solid was filtered
- washwashed with water