HRID844024

反应详情

EQUATION

反应方程式

HRID 844024 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
220 °C

PROCEDURE

实验过程

A mixture of 1-(3-chloro-5-methoxy-phenyl)-ethanone (14.3 g, 0.08 mol.) and pyridine hydrochloride (44.8 g, 0.39 mol.) was heated at 220° C. for 2 hrs. The mixture was poured into water (200 mL) and extracted with ethyl acetate (2×200 mL). The organic extracts were combined, washed with water (40 mL), brine (40 mL) and concentrated to give an oil. Flash Chromatography on Silica Get eluting with ethyl acetate/hexanes (1:1) gave 6.6 g solid. MS (m/e): 170/172 (M+).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (2×200 mL)
  2. washwashed with water (40 mL), brine (40 mL)
  3. concentrationconcentrated
  4. customto give an oil
  5. customFlash Chromatography on Silica Get
  6. washeluting with ethyl acetate/hexanes (1:1)