HRID647406

反应详情

EQUATION

反应方程式

HRID 647406 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 10 ml of acetone was dissolved 1.5 g of 2-(4-chloro-2-fluorophenyl)-2,3,4,5,6,7-hexahydro-3-mercapto-1H-isoindol-1-one, and 1.5 g of methyl iodide and 1.3 g of potassium carbonate were added to the solution, followed by stirring at 40° to 50° C. for 5 hours. After cooling, the insoluble matter was filtered out, and the filtrate was concentrated under reduced pressure. The residual, oily substance was purified by means of column chromatography with the use of silica gel (developing solvent of acetone-hexane), thereby producing 1.4 g (yield of 90%) of the subject compound in white crystals, m.p. 97°-98° C.

WORKUP

后处理

  1. additionwere added to the solution
  2. temperatureAfter cooling
  3. filtrationthe insoluble matter was filtered out
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residual, oily substance was purified by means of column chromatography with the use of silica gel (developing solvent of acetone-hexane)