HRID280620

反应详情

EQUATION

反应方程式

HRID 280620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7-bromo-1-tetralone (11.25 g), pyridin-3-carboxaldehyde (5.35 g), acetic acid (5 ml) and piperidine (6 ml) was heated on a steam bath for 6 hours and then allowed to stand for 18 hours. The volatile material was evaporated and the residue was dissolved in ethyl acetate. The solution was extracted several times with dilute hydrochloric acid and the combined extracts were made just alkaline with dilute sodium hydroxide solution. The solid was filtered off, washed with water and crystallised from methanol to give 7-bromo-2-(3-pyridylmethylene)-1-tetralone (12.8 g), m.p. 124°-125°.

WORKUP

后处理

  1. temperaturewas heated on a steam bath for 6 hours
  2. customThe volatile material was evaporated
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. extractionThe solution was extracted several times with dilute hydrochloric acid
  5. filtrationThe solid was filtered off
  6. washwashed with water
  7. customcrystallised from methanol