HRID510091
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
- 0 °C
PROCEDURE
实验过程
300 mg (0.768 mmol) of the compound from example 41 and 211 mg (0.768 mmol) of BEMP were initially charged in 10 ml of dimethylformamide, and a solution of 109 mg (0.768 mmol) of iodomethane in 2 ml of dimethylformamide was added dropwise at 0° C. within 10 min. The mixture was stirred at 0° C. for 3 h. Water was added, which formed a precipitate. The precipitate was filtered off and purified by means of preparative HPLC (eluent: methanol/water, gradient 30:70→90:10). 203 mg of the title compound were obtained (65% of theory).
WORKUP
后处理
- customwhich formed a precipitate
- filtrationThe precipitate was filtered off
- custompurified by means of preparative HPLC (eluent: methanol/water, gradient 30:70→90:10)