HRID922734

反应详情

EQUATION

反应方程式

HRID 922734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 20 ml of methylene chloride, 1.00 g of Compound 2-1 obtained in Production Example 1 was dissolved. To the solution thus obtained, 0.68 ml of triethylamine and 0.324 ml of methanesulfonyl chloride were added. Thereafter, the resulting mixture was stirred at room temperature for 1.5 hours. After the reaction, water was added to the reaction solution thus obtained, and extraction with ethyl acetate was then carried out. The organic layer thus extracted was washed with an aqueous solution of sodium hydrogen carbonate 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 1.141 g of Compound 3-1-1.

WORKUP

后处理

  1. dissolutionwas dissolved
  2. customTo the solution thus obtained
  3. additionwas added to the reaction solution
  4. customthus obtained
  5. extractionextraction with ethyl acetate
  6. extractionThe organic layer thus extracted
  7. washwas washed with an aqueous solution of sodium hydrogen carbonate and saturated brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. distillationThe solvent was distilled away
  10. customthe residue was then purified by silica gel column chromatography