反応 #2488

反応方程式

2-propanol

4-methyl-4'-chlorodiphenylsulfone

thioglycolic acid

potassium hydroxide

→

4-(4-methylphenylsulfonyl)phenylthio acetic acid

溶媒

water

N,N-dimethylformamide

反応条件

後処理

1. 1
   ろ過filtered off
2. 2
   その他to obtain a precipitate
3. 3
   その他After the precipitate obtained
4. 4
   ろ過the insoluble matter was filtered off
5. 5
   workup.ADDITION150 ml of concentrated chloric acid and 500 g of ice were added
6. 6
   ろ過The formed white crystal was filtered off
7. 7
   洗浄washed with water
8. 8
   その他further recrystallized with a mixed solvent of n-hexane and ethylacetate

実験手順

In 250 ml of N,N-dimethylformamide, 140 g of 4-methyl-4'-chlorodiphenylsulfone was dissolved, and further 77 g of thioglycolic acid and 71 g of 85% potassium hydroxide pellet were added and stirred for 6 hours at 120° C. The reaction mixture was poured into 2-propanol and filtered off to obtain a precipitate. After the precipitate obtained was dissolved in water and then the insoluble matter was filtered off, 150 ml of concentrated chloric acid and 500 g of ice were added therein. The formed white crystal was filtered off and washed with water and further recrystallized with a mixed solvent of n-hexane and ethylacetate to obtain 110 g of the intended 4-(4-methylphenylsulfonyl)phenylthio acetic acid.

出典