HRID931150

反应详情

EQUATION

反应方程式

HRID 931150 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of cyclopropanecarboxamide (3.5 g, 41.46 mmol) in toluene and 1,4-dioxane (50 mL, 1:1) was added ethyl 4-chloro-3-oxobutanoate (20.0 g, 121.95 mmol). The mixture was heated to 100° C. for 18 h, then was diluted with water and extracted with ethyl acetate. The organic layer was dried and concentrated under reduced pressure. The crude material was purified via column chromatography on 100-200 mesh silica (20% ethyl acetate in petroleum ether) to afford ethyl 2-(2-cyclopropyloxazol-4-yl)acetate (3.5 g). MS (ES+APCI) 196.1; LCMS retention time: 4.029 min (Method Q1).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. customThe organic layer was dried
  3. concentrationconcentrated under reduced pressure
  4. customThe crude material was purified via column chromatography on 100-200 mesh silica (20% ethyl acetate in petroleum ether)