反応 #6604

反応方程式

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

反応条件

後処理

1. 1
   温度cooled to room temperature
2. 2
   抽出extracted with ether
3. 3
   洗浄The organic phase was washed
4. 4
   乾燥dried over magnesium sulfate
5. 5
   その他evaporated under reduced pressure
6. 6
   その他Recrystallization of the residue from methanol

実験手順

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.

出典