HRID2300589

反应详情

EQUATION

反应方程式

HRID 2300589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Intermediate 1E was prepared (as described below for the preparation of intermediate 2B) from 4.08 g of benzamide, 5.0 g of ethyl 3-bromo-2-oxo-pentanoate, and 10 mL of toluene. Solids were collected and washed with cold water after cooling of the NaOH solution. Heating these solids with citric acid as described followed by cooling and isolation of the resulting solids gave 410 mg (9% yield) of the title compound; 1H NMR (CDCl3, 300 MHz) δ8.06-8.03 (m, 2H), 7.49-7.43 (m, 3H), 3.14 (q, 2H, J=8.0), 1.34 (t, 3H, J=8.0); low resolution MS (ES+)m/e 217.8 (MH+).

WORKUP

后处理

  1. customIntermediate 1E was prepared (
  2. customSolids were collected
  3. washwashed with cold water
  4. temperatureafter cooling of the NaOH solution
  5. temperatureHeating these solids with citric acid
  6. temperatureby cooling