HRID1736716

反应详情

EQUATION

反应方程式

HRID 1736716 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 32.62 g of 2,4-difluoronitrobenzene, 24.2 g of 2-aminoisobutyric acid, 15.2 g of potassium carbonate, 100 ml of acetonitrile, and 100 ml of water is heated at 80° for 2 days (until TLC shows little or no starting material). The reaction is then cooled and acetonitrile is removed under reduced pressure. The pH is adjusted to 5 with 4N hydrochloric acid and the mixture is extracted with chloroform (3×300 ml). The organic layers are dried over sodium sulfate and concentrated. The material is used in the next step without further purification.

WORKUP

后处理

  1. temperatureis heated at 80° for 2 days (until TLC
  2. temperatureThe reaction is then cooled
  3. customacetonitrile is removed under reduced pressure
  4. extractionthe mixture is extracted with chloroform (3×300 ml)
  5. dry with materialThe organic layers are dried over sodium sulfate
  6. concentrationconcentrated
  7. customThe material is used in the next step without further purification