HRID484497
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
- 145 °C
PROCEDURE
实验过程
A mixture of 10.7 parts of methyl 4-[[4-hydroxy-1-(phenylmethyl)-4-piperidinyl]methoxy]benzoate and 8 parts of 2-aminoethanol was stirred for 4 hours in an oil bath at 145° C. After cooling, the reaction mixture was poured into water. The oil was decanted, washed twice with water and the product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was crystallized from a mixture of 2,2-oxybispropane and 2-propanol. The product was filtered off and dried yielding 8 parts (69.3%) of N-(2-hydroxyethyl)-4-[[4-hydroxy-1-(phenylmethyl)-4-piperidinyl]methoxy]benzamide; mp. 161.1° C. (int. 80).
WORKUP
后处理
- temperatureAfter cooling
- customThe oil was decanted
- washwashed twice with water
- extractionthe product was extracted with dichloromethane
- customThe extract was dried
- filtrationfiltered
- customevaporated
- customThe residue was crystallized from a mixture of 2,2-oxybispropane and 2-propanol
- filtrationThe product was filtered off
- customdried