HRID1888263
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
- 100 °C
PROCEDURE
实验过程
To a solution of 3-{1-[(3-chloropropyl)sulfonyl]-4-piperidinyl}-5-(3-fluorophenyl)-1H-indazole-7-carboxamide (0.222 mmol) in DMF (4 mL) was added K2CO3 (61 mg, 0.444 mmol) and diethyl amine (115 uL, 1.11 mmol). The reaction mixture was heated to 100° C. overnight. The solution was filtered and the filtrate was purified by using a Gilson semi-preparative HPLC system with a YMC ODS-A (C-18) column 50 mm by 20 mm ID, eluting with 10% B to 80% B in 10 min, hold for 1 min where A=H2O (0.1% trifluoroacetic acid) and B=CH3CN (0.1% trifluoroacetic acid) pumped at 25 mL/min to afford the title compound (24.7 mg, 22% for 2 steps).
WORKUP
后处理
- filtrationThe solution was filtered
- customthe filtrate was purified
- washeluting with 10% B to 80% B in 10 min