HRID5357

反应详情

EQUATION

反应方程式

HRID 5357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3.00 g (11.4 mmol) of ethyl 2,3,4,5-tetrafluorobenzoylacetate, 870 mg (11.4 mmol) of carbon disulfide and 9 ml of dried dimethyl sulfoxide were added 2.31 g (22.8 mmol) of triethylamine at room temperature, and the mixture was stirred for 1 hour at room temperature. Then, at room temperature, 3.24 g (22.8 mmol) of methyl iodide were added and the mixture was stirred for 2 hours, which was poured into ice-water. The crystals deposited were collected by filtration and dried to obtain 2.81 g (8.41 mmol) of title compound (yield 74%.

WORKUP

后处理

  1. stirringthe mixture was stirred for 2 hours
  2. filtrationThe crystals deposited were collected by filtration
  3. customdried