反应详情

A mixture of 12.1 parts of dimethyl (tetrahydro-3,3-diphenyl-2-furylidene) ammonium bromide, 8.4 parts of 4-(4-chloro-3-trifluoromethylphenyl)-4-piperidinol, 8 parts of sodium carbonate, 0.4 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed for 3 hours with water separator. The reaction mixture is cooled and water is added. The organic layer is separated, washed with diluted sodium hydroxide solution, dried and concentrated to a volume of about 200 parts. The concentrate is acidified with an excess of 2-propanol previously saturated with gaseous hydrogen chloride. Upon stirring, the salt is crystallized. It is filtered off and dried, yielding 4-(4-chloro-3-trifluoromethylphenyl)-4-hydroxy-N,N-dimethyl-α,α-diphenylpiperidine-1 -butyramide hydrochloride; m.p. 215.3° C.

1. temperatureThe reaction mixture is cooled
2. customThe organic layer is separated
3. washwashed with diluted sodium hydroxide solution
4. customdried
5. concentrationconcentrated to a volume of about 200 parts
6. stirringUpon stirring
7. customthe salt is crystallized
8. filtrationIt is filtered off
9. customdried