تفاعل #6604

معادلة التفاعل

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

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled to room temperature
2. 2
   استخلاصextracted with ether
3. 3
   غسيلThe organic phase was washed
4. 4
   تجفيفdried over magnesium sulfate
5. 5
   أخرىevaporated under reduced pressure
6. 6
   أخرىRecrystallization of the residue from methanol

الإجراء التجريبي

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.

المصدر