反应详情

温度

60 °C

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 1 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.

1. temperaturecooled to room temperature
2. additionpoured into 1.5 1 of ice
3. extractionextracted with ether
4. washThe organic phase was washed
5. dry with materialdried over magnesium sulfate
6. customevaporated under reduced pressure
7. customRecrystallization of the residue from methanol