HRID2073191
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
To a solution of 100 mg of 4,5-dihydro-5-thioxo-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one (Example 8) in 10 ml of dry tetrahydrofuran, cooled at 0° C., was added 13 mg of sodium hydride (60% dispersion in mineral oil). The reaction mixture was stirred at 0° C. for 15 minutes, then an excess of methyl iodide was added. The mixture was allowed to warm to room temperature then was stirred for 3 hours. The mixture was quenched with water and extracted with chloroform. Evaporation of the extract in vacuo gave 47 mg of the product of the example as a yellow solid, m.p. 234°-237° C. (dec).
WORKUP
后处理
- temperatureto warm to room temperature
- stirringthen was stirred for 3 hours
- customThe mixture was quenched with water
- extractionextracted with chloroform
- customEvaporation of the
- extractionextract in vacuo