反应详情

温度

-10 °C

4-(2-Chloroethylsulfanyl)-benzoic acid (18.4 mmol) is suspended in methylene chloride (60 ml) and cooled to −10C. m-Chloroperbenzoic acid (38.6 mmol) are added dropwise in methylene chloride (60 ml) and the mixture is stirred for e hours at −10° C. The mixture is diluted methylene chloride (100 ml) and a 5% solution of sodium thiosulfate in water is added and the mixture vigorously stirred. The mixture is extracted, washed with water and and dried over sodium sulfate and evaporated. The crude product is recrystallized from ethylacetate and the solid filtered of and dried (vacuum). 2.19 g of a pale powder with mp. 142-144° C., Rf=0.37 (CH2Cl2/MeOH=9:1) is obtained.

1. temperaturecooled to −10C
2. stirringthe mixture vigorously stirred
3. extractionThe mixture is extracted
4. washwashed with water
5. dry with materialdried over sodium sulfate
6. customevaporated
7. customThe crude product is recrystallized from ethylacetate
8. filtrationthe solid filtered of and
9. customdried (vacuum)