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
PROCEDURE
实验过程
1.64 g of dicyclohexylcarbodiimide dissolved in 20 ml of chloroform are added at room temperature to 1.5 g of (R/S)-2-(3-acetoxy-2-oxo-1-pyrrolidinyl)acetic acid, 40 ml of chloroform and 0.86 g of N-hydroxysuccinimide. After 4 hours, the solid is filtered, whereupon the filtrate is concentrated and again filtered. The filtrate is evaporated. The residue is treated at room temperature with 40 ml of a saturated solution of ammonia in methanol. The mixture is stirred at room temperature for 5 minutes, 10 ml of ion-free water are then added thereto and the mixture is stirred at room temperature for an additional minutes. The precipitated solid is filtered. The filtrate is evaporated, the residue is stirred in 30 ml of acetonitrile and the crystallized-out product is recrystallized two more times from acetonitrile. There is obtained (R/S)-2-(3-hydroxy-2-oxo-1-pyrrolidinyl)acetamide of melting point 162°-164°.
WORKUP
后处理
- filtrationthe solid is filtered, whereupon the filtrate
- concentrationis concentrated
- filtrationagain filtered
- customThe filtrate is evaporated
- additionThe residue is treated at room temperature with 40 ml of a saturated solution of ammonia in methanol
- addition10 ml of ion-free water are then added
- stirringthe mixture is stirred at room temperature for an additional minutes
- filtrationThe precipitated solid is filtered
- customThe filtrate is evaporated
- stirringthe residue is stirred in 30 ml of acetonitrile
- customthe crystallized-out product is recrystallized two more times from acetonitrile