반응 #6604

반응 방정식

1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene

chlorosulfonic acid

→

5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene-2-sulfonyl chloride

반응 조건

후처리

1. 1
   온도cooled to room temperature
2. 2
   추출extracted with ether
3. 3
   세척The organic phase was washed
4. 4
   건조dried over magnesium sulfate
5. 5
   기타evaporated under reduced pressure
6. 6
   기타Recrystallization of the residue from methanol

실험 절차

94.0 g (0.5 mol) of 1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene were stirred into 100 ml of chlorosulfonic acid at 20° C. within 30 min. The reaction solution was maintained at 60° C. for 1 hour, cooled to room temperature and then poured into 1.5 l of ice and extracted with ether. The organic phase was washed to neutrality with brine and water, dried over magnesium sulfate and evaporated under reduced pressure. Recrystallization of the residue from methanol yielded 55.0 g of 5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene-2-sulfonyl chloride of melting point 71°-74° C.

출처