반응 #5980

반응 방정식

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

용매

water

chloroform

chloroform

chloroform

반응 조건

후처리

1. 1
   workup.STIRRINGStirring
2. 2
   workup.WAITis continued overnight
3. 3
   기타the two layers separated
4. 4
   세척the chloroform layer washed twice with water
5. 5
   건조dried over magnesium sulfate
6. 6
   여과filtered
7. 7
   기타evaporated to dryness

실험 절차

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.

출처