反应 #5980

反应方程式

ethylchloroformate

3-aminoquinuclidine dihydrochloride

1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylic acid

triethylamine

→

1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran

溶剂

water

chloroform

chloroform

chloroform

反应条件

后处理

1. 1
   workup.STIRRINGStirring
2. 2
   workup.WAITis continued overnight
3. 3
   其他the two layers separated
4. 4
   洗涤the chloroform layer washed twice with water
5. 5
   干燥dried over magnesium sulfate
6. 6
   过滤filtered
7. 7
   其他evaporated to dryness

实验过程

To a cold solution of 0.3 g 1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylic acid in 40 ml chloroform is added 0.3 g of triethylamine and then 0.2 g ethylchloroformate in 10 ml chloroform. Stirring is continued for 2 hours. This is then added to a cold mixture of 3 g 3-aminoquinuclidine dihydrochloride in 20 ml water containing 7.5 g K2CO3. Stirring is continued overnight. The reaction mixture is then diluted with chloroform, the two layers separated and the chloroform layer washed twice with water, dried over magnesium sulfate, filtered and evaporated to dryness to give 1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-(N-1-azabicyclo [2.2.2.]oct-3-yl)carboxamide as an oily Product.

来源