反应详情

The procedure of Example 3 was repeated, except that the Grignard reagent was prepared from 2.0 g of magnesium turnings and 10.3 g of 1-methyl-3-chloromethylpiperidine and the use of iodine was omitted, the 4-fluorobenzonitrile was replaced with 13.3 g of 3,4-dichlorobenzonitrile, the ammonium chloride solution was replaced with 100 ml of water containing 8 of ammonium chloride, the work-up procedure generally followed that described in Example 2, and the maleate salt procedure was not employed. The crude product, 16.2 g, was recrystallized first from acetone and then from hexane to give 7.4 g of 1-methyl-3-(3,4-dichlorophenacyl)piperidine, mp 69°-71°. The following elemental analysis was obtained:

1. customThe crude product, 16.2 g, was recrystallized first from acetone