反応 #1120022

反応方程式

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

triethylamine

dihydrochloride

ethylchloroformate

→

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

溶媒

chloroform

water

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
   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-aminoguinuclidine dihydrochloride in 20 ml water containing 7.5 g K2CO3. Stirring is continued overnight. The reaction mxiture is then diluted with chloroform, the two layers separated and the chloroform layer washed twice with water, dried over magnesium sulfate and evaporated to dryness to give 1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-(N-1-azabicylo[2.2.2.]oct-3-yl]carboxamide as an oily product.

出典