HRID922735

反应详情

EQUATION

反应方程式

HRID 922735 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 95 ml of toluene, 4.756 g of Compound 2-1 obtained in Production Example 1 was dissolved. To the solution thus obtained, 3.12 ml of triethylamine and 1.76 ml of N-methylimidazole were added, and 3.38 g of 4-toluenesulfonyl chloride was added. The resulting mixture was stirred at room temperature for 100 minutes. After the reaction, water was added to the reaction solution thus obtained, and the organic layer was separated from the suspension. Thereafter, the aqueous layer was extracted with toluene and then blended with the organic layer previously obtained. The resultant organic layer thus obtained was washed with an aqueous solution of 1 mol/l hydrochloric acid and saturated brine and then dried over anhydrous sodium sulfate. The solvent was distilled away, and the residue was then purified by silica gel column chromatography to obtain 5.397 g of Compound 3-1-2.

WORKUP

后处理

  1. dissolutionwas dissolved
  2. customTo the solution thus obtained
  3. additionwas added to the reaction solution
  4. customthus obtained
  5. customthe organic layer was separated from the suspension
  6. extractionThereafter, the aqueous layer was extracted with toluene
  7. custompreviously obtained
  8. customThe resultant organic layer thus obtained
  9. washwas washed with an aqueous solution of 1 mol/l hydrochloric acid and saturated brine
  10. dry with materialdried over anhydrous sodium sulfate
  11. distillationThe solvent was distilled away
  12. customthe residue was then purified by silica gel column chromatography