HRID922739

反应详情

EQUATION

反应方程式

HRID 922739 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To 1.00 g of Compound 3-1-3 synthesized in Production Example 4, 0.578 g of toluenesulfonic acid monohydrate and 100 mg of water were added, and the resulting mixture was stirred in an oil bath of 120° C. 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 extract was washed with an aqueous solution of sodium hydrogen carbonate and saturated brine. After the organic layer was dried over anhydrous sodium sulfate, the solvent was distilled away. The residue was purified by silica gel column chromatography to obtain 752 mg of Compound 4-1-3.

WORKUP

后处理

  1. additionwere added
  2. additionwas added to the reaction solution
  3. customthus obtained
  4. extractionextraction with ethyl acetate
  5. washThe extract was washed with an aqueous solution of sodium hydrogen carbonate and saturated brine
  6. dry with materialAfter the organic layer was dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled away
  8. customThe residue was purified by silica gel column chromatography