HRID1534478

反应详情

EQUATION

反应方程式

HRID 1534478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Diphenyl ether (500 ml) was heated to reflux, ethyl 2-isobutyryl-3-(2-(benzoyloxymethyl)phenylaminoacrylate (29.3 g, 74.1 mmol) added, and heating continued for 15 minutes. The bulk of the diphenyl ether was removed by vacuum distillation, and the residue chromatographed (silica gal, 1%-2.5% methanol in dichloromethane) and recrystallized from ethyl acetate to give 3-isobutyryl-8-benzoyloxymethyl)-4(1H)-quinolone (11.9 g, 46%), m.p. 158°-160°.

WORKUP

后处理

  1. temperatureto reflux
  2. temperatureheating
  3. customThe bulk of the diphenyl ether was removed by vacuum distillation
  4. customthe residue chromatographed (silica gal, 1%-2.5% methanol in dichloromethane)
  5. customrecrystallized from ethyl acetate