HRID1018976

反应详情

EQUATION

反应方程式

HRID 1018976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-methylene-3-quinuclidinone dihydrate hydrochloride (25.7 g, 0.1225 mol, 1 eq) and K2CO3 (67.0 g, 0.4848 mol, 4 eq) is dissolved in 125 mL water and 200 mL CH2Cl2 and stirred vigorously. After 16 h, the layers are separated and the aqueous layer is extracted with CH2Cl2. The combined organic layers are dried over MgSO4, filtered and concentrated to give 14.75 g (88%) of 2-methylenequinuclidin-3-one as a yellow oil. MS (ESI) for C8H11NO m/z 138.1 (M+H)30 .

WORKUP

后处理

  1. customthe layers are separated
  2. extractionthe aqueous layer is extracted with CH2Cl2
  3. dry with materialThe combined organic layers are dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated