HRID1085781

反应详情

EQUATION

反应方程式

HRID 1085781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 25 ml of N,N-dimethylformamide were added 12 g of diiodoethane and 8.3 g of potassium carbonate, a solution of 6.07 g of the compound obtained in Example 4 dissolved in 60 ml of N,N-dimethylformamide was gradually dropped thereinto, and the mixture was stirred for 30 minutes at the same temperature. N,N-Dimethylformamide was evaporated therefrom in vacuo, the residue was dissolved in a mixture of chloroform and methanol (2:1), washed with water, dried over magnesium sulfate, the solvent was evaporated therefrom, and the crystals separated out therefrom were washed with ether to give 3.35 g of ethyl 6,7,8-trifluoro-1-methyl-4-oxo-4H-[1,3]thiazeto[3,2-a]quinoline-3-carboxylate.

WORKUP

后处理

  1. additionwas gradually dropped
  2. customN,N-Dimethylformamide was evaporated
  3. dissolutionin vacuo, the residue was dissolved in a mixture of chloroform and methanol (2:1)
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. customthe solvent was evaporated
  7. customthe crystals separated
  8. washout therefrom were washed with ether