HRID1018549
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
Sodium hydride (34 mg, 60%) was suspended in N-methyl-2-pyrrolidone (2 mL) and 8-(3,5-bis-trifluoromethyl-benzoyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one (200 mg) was added with stirring. After 5 minutes stirring at room temperature 4-(2-chloroethyl)morpholine hydrochloride (79 mg) was added. The mixture was heated to 100° C. with stirring and kept for 1 h at that temperature. After cooling, saturated sodium bicarbonate solution was added and the mixture was extracted with ethylacetate. Organic phases were pooled, dried with Na2SO4 and the solvent was evaporated. Chromatography on silica gel (ethylacetate) yielded the desired product (180 mg, 73%), MS: m/e=585.1 (M+H+).
WORKUP
后处理
- additionwas added
- stirringwith stirring
- temperatureAfter cooling
- extractionthe mixture was extracted with ethylacetate
- dry with materialdried with Na2SO4
- customthe solvent was evaporated