HRID2263376

反应详情

EQUATION

反应方程式

HRID 2263376 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1.5 g of [4-(3-benzyloxy-propyl)-2-(4-trifluoromethyl-phenyl)-thiazol-5-yl]-methanol in 15 mL of dichloromethane was added 1.026 mL of triethylamine and 0.484 mL of methanesulfonyl chloride. The resulting mixture was stirred at room temperature for 2 h. The mixture was then diluted with dichloromethane and water was added. The aqueous layer was separated and extracted three times with dichloromethane. The combined organic extracts were washed with water, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel (heptane 90/ethyl acetate 10) to give 0.84 g of 4-(3-benzyloxy-propyl)-5-chloromethyl-2-(4-trifluoromethyl-phenyl)-thiazole as a yellow oil.

WORKUP

后处理

  1. additionwas added
  2. customThe aqueous layer was separated
  3. extractionextracted three times with dichloromethane
  4. washThe combined organic extracts were washed with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe crude product was purified by column chromatography on silica gel (heptane 90/ethyl acetate 10)