反应 #84048

ord-0186fe48a824439e807128658024c08c

反应方程式

Cl.O=C1CN2CCC1CC2
quinuclidin-3-one hydrochloride
C[O-].[Na+]
sodium methoxide
O=C1CN2CCC1CC2
title compound
O=C1CN2CCC1CC2
Quinuclidin-3-one

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The resulting precipitate is filtered off with suction
  2. 2
    浓缩the filtrate is concentrated in vacuo
  3. 3
    其他The residue is partitioned between chloroform and water
  4. 4
    萃取extracted with chloroform
  5. 5
    干燥The combined organic phases are dried over sodium sulfate
  6. 6
    浓缩concentrated in vacuo

实验过程

100 g (0.62 mol) of quinuclidin-3-one hydrochloride are suspended in 2 l of methanol. At 0° C., a solution of 33.4 g (0.62 mol) of sodium methoxide in 250 ml of methanol is slowly added dropwise. The mixture is stirred at room temperature for 16 h. The resulting precipitate is filtered off with suction, and the filtrate is concentrated in vacuo. The residue is partitioned between chloroform and water and extracted with chloroform. The combined organic phases are dried over sodium sulfate and concentrated in vacuo. 58.8 g (75.9% of theory) of the title compound are obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09433614B2uspto-grants-2016_09