反应详情

A stirred suspension of 1.7 g. (0.02 mole) of piperidine and 5.8 g. (0.02 mole) of 2,4-dichloro-5-chlorosulfonylbenzoic acid (Sturm, et al., Ber., 99, 328 (1966) in 70 ml. of water and cooled to 15° C. is treated dropwise with 50 ml. of 1N sodium hydroxide. When the addition is complete, the mixture is allowed to warm to room temperature and remain for 1 hr. The hazy suspension is filtered and the clear filtrate acidified with 12N hydrochloric acid. The precipitated solids are filtered and dried, 7.7 g., m.p. 200°-205° C. A sample is recrystallized from acetonitrile, m.p. 205°-206° C.

1. additionA stirred suspension of 1.7 g
2. additionis treated dropwise with 50 ml
3. additionWhen the addition
4. filtrationThe hazy suspension is filtered
5. filtrationThe precipitated solids are filtered
6. customdried
7. customA sample is recrystallized from acetonitrile, m.p. 205°-206° C.