反应详情

温度

40 °C

20.6 g (0.1 mole) of 2,5-dichloro-3-aminobenzoic acid and 18.7 g (0.12 mole) of hydroxymethyl-(β-chloroethyl)-sulfone were suspended in 100 ml of ethylene chloride, 1 ml of concentrated sulfuric acid was added thereto and the mixture was stirred for 3 hours at 40° C. The mixture was then cooled and the product which had crystallized out was filtered off and recrystallized from acetonitrile. This gave 30.8 g (89% of theory) of 2,5-dichloro-3-[(β-chloroethyl)-sulfonylmethylamino]-benzoic acid in the form of colorless crystals of melting point 156° C (with decomposition).

1. temperatureThe mixture was then cooled
2. customthe product which had crystallized out
3. filtrationwas filtered off
4. customrecrystallized from acetonitrile