反应 #2488

ord-ceb80269f1a342758c971e5e753be1b3

反应方程式

CC(C)O
2-propanol
Cc1ccc(S(=O)(=O)c2ccc(Cl)cc2)cc1
4-methyl-4'-chlorodiphenylsulfone
O=C(O)CS
thioglycolic acid
[K+].[OH-]
potassium hydroxide
Cc1ccc(S(=O)(=O)c2ccc(CC(O)=S)cc2)cc1
4-(4-methylphenylsulfonyl)phenylthio acetic acid

反应条件

温度
120°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05728879uspto-grants-1998_03