反应详情

温度

50 °C

31.7 g (0.091 mol) of p-chlorobenzylmercaptoacetohydroxamic acid are mixed with 100 ml of anhydrous acetic acid and 9.1 ml of hydrogen peroxide of 110 volumes strength are added. The temperature, which is 20° C. at the start, rises and solution of the precipitate formed is also observed. The temperature is maintained at 50° C. and after several minutes it is found that the sulphinyl derivative sets solid. 50 ml of acetic acid are now added and the temperature is kept at 50° C. for 1 hour whilst stirring vigorously. The mixture is cooled and the p-chlorobenzylsulphinyl-acetohydroxamic acid is filtered off. This acid is recrystallised from acetic acid and filtered off, the precipitate is washed with water and with ethanol, and dried, and 31.9 g of CRL 40,411 are collected. Yield 85%; instantaneous melting point 210° C. (with decomposition).

1. additionare added
2. customis 20° C. at the start
3. customsolution of the precipitate formed
4. temperatureThe mixture is cooled
5. filtrationthe p-chlorobenzylsulphinyl-acetohydroxamic acid is filtered off
6. customThis acid is recrystallised from acetic acid
7. filtrationfiltered off
8. washthe precipitate is washed with water and with ethanol
9. customdried
10. custom31.9 g of CRL 40,411 are collected