反応 #5980

反応方程式

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

溶媒

water

chloroform

chloroform

chloroform

反応条件

後処理

1. 1
   workup.STIRRINGStirring
2. 2
   workup.WAITis continued overnight
3. 3
   その他the two layers separated
4. 4
   洗浄the chloroform layer washed twice with water
5. 5
   乾燥dried over magnesium sulfate
6. 6
   ろ過filtered
7. 7
   その他evaporated to dryness

実験手順

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.

出典