HRID347657

反应详情

EQUATION

反应方程式

HRID 347657 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 (27.2 g, 0.13 mol, 1 eq) and K2CO3 (86.0 g, 0.62 mol, 4.8 eq) is dissolved in 130 mL water and 250 mL CH2Cl2 and stirred vigorously. After 3 days, the layers are separated and the aqueous layer is extracted with CH2Cl2. The combined organic layers are dried (MgSO4), filtered and concentrated to give 17.8 g (100%) of 2-methylenequinuclidin3-one as a yellow oil. MS (ESI) for C8H11NO m/z 138.1 (M+).

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 (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated