反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred solution of 1.5 g of {4-[3-(benzyloxy)propyl]-2-[4-(trifluoromethyl)phenyl]-1,3-thiazol-5-yl}methanol in 15 mL of dichloromethane were added 0.484 g of methanesulfonylchloride and 1.03 mL of triethylamine. The solution was stirred for 2 h at room temperature. The mixture was diluted with dichloromethane and poured into water. The aqueous layer was separated and extracted three times with dichloromethane. The combined organic layers were dried over magnesium sulfate, filtered and concentrated under reduced pressure to give 1.65 g of crude product as a yellow oil. Purification by column chromatography on silica gel (heptane 90/ethyl acetate 10) gave 0.840 g of 4-(3-benzyloxy-propyl)-5-chloromethyl-2-(4-trifluoromethyl-phenyl)-thiazole.
WORKUP
后处理
- customThe aqueous layer was separated
- extractionextracted three times with dichloromethane
- dry with materialThe combined organic layers were dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customto give 1.65 g of crude product as a yellow oil
- customPurification by column chromatography on silica gel (heptane 90/ethyl acetate 10)