반응 #1942895

반응 방정식

sodium chloride

water

N-acetyl-4,5,6,7-tetrahydrobenzo[b]thiophen-4-amine

water

→

title compound

N-Acetyl-4,5,6,7-tetrahydro-7-oxobenzo[b]-thiophen-4-amine

용매

acetic anhydride

acetic acid

반응 조건

후처리

1. 1
   workup.WAITAfter an hour at 20° C.
2. 2
   추출extracted with trichloromethane (100, 150 and 50 ml volumes)
3. 3
   추출The combined extract
4. 4
   세척is washed with brine
5. 5
   세척The water wash
6. 6
   추출is extracted with trichloromethane
7. 7
   추출extract
8. 8
   기타Evaporation of the extract
9. 9
   기타affords a yellow-green residue, which after trituration with ether

실험 절차

A solution of 2.15 g of N-acetyl-4,5,6,7-tetrahydrobenzo[b]thiophen-4-amine in 12 ml of acetic acid is stirred and 3.04 g of chromium trioxide in 13.6 ml of acetic anhydride is added in 15 minutes at 10° C. to 15° C. After an hour at 20° C., 20 ml of water is added and the mixture is allowed to stand overnight. Additional water (50 ml) is added, the mixture is saturated with sodium chloride and extracted with trichloromethane (100, 150 and 50 ml volumes). The combined extract is washed with brine and then with water. The water wash is extracted with trichloromethane and the extract is combined with the main trichloromethane extract. Evaporation of the extract affords a yellow-green residue, which after trituration with ether gives 1.32 g of the title compound, m.p. 160° C. to 164° C.

출처