HRID1413947

反应详情

EQUATION

反应方程式

HRID 1413947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 27.39 g (0.25 mole) of ethyl formimidate hydrochloride [prepared by the method of Ohme, et al., Angew. Chem. Intl. Ed., 6, 566(1967)] and 52.71 g (0.20 mole) of diphenyl-4-piperidylmethane in 80 ml of freshly-opened absolute ethanol was stirred magnetically under a calcium chloride tube overnight. The suspension was filtered and diethylether was added to the filtrate. The filtrate was stripped to dryness and the resulting oil was crystallized from isopropanol. The solid was then suspended in boiling ethyl acetate to obtain a higher melting form. Two recrystallizations from ethanol-ether yielded pure 4-diphenylmethyl-1-iminomethylpiperidine hydrochloride hydrate; m.p. 220°-221° C.

WORKUP

后处理

  1. customprepared by the method of Ohme, et al., Angew
  2. filtrationThe suspension was filtered
  3. additiondiethylether was added to the filtrate
  4. customthe resulting oil was crystallized from isopropanol
  5. customto obtain
  6. customTwo recrystallizations from ethanol-ether yielded pure 4-diphenylmethyl-1-iminomethylpiperidine hydrochloride hydrate