反应详情

To cis-3,5-dimethylpiperidine (374 mg.; 3.3 m moles) in 3 ml. of methylene chloride is added 192 mg. (0.66 m moles) of 2,3-dichloro-5-chlorosulfonylbenzoic acid and the mixture heated to reflux for 1.5 hrs. The solvent is removed under reduced pressure, and the residue is partitioned between 25 ml. of 1 N sodium hydroxide solution and diethyl ether. The aqueous layer is separated, acidified with 6 N hydrochloric acid and the resulting precipitated product filtered and dried, 230 mg., m.p. 235°-238° C. Recrystallization from acetonitrile gave the purified product, m.p. 244°-245° C.

1. temperatureto reflux for 1.5 hrs
2. customThe solvent is removed under reduced pressure
3. customthe residue is partitioned between 25 ml
4. customThe aqueous layer is separated
5. customthe resulting precipitated product
6. filtrationfiltered
7. customdried
8. customRecrystallization from acetonitrile
9. customgave the purified product, m.p. 244°-245° C.