HRID41591
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 (2-methyl-5-m-tolylthiazol-4-yl)methanol (300 mg, 1.37 mmol) in chloroform (10 mL), thionyl chloride (162 mg, 1.37 mmol) was added dropwise at rt and stirred for 30 min and then refluxed for 1 h. The reaction mixture was cooled to rt and absorbed directly on silicagel (10 g). Subsequent flash column chromatography (eluent: 7% ethyl acetate in hexane) yielded the title compound (40 mg, 12%). [LCMS RtF=1.70 min, [M+H]+=238.0; TLC Rf=0.54 (methanol/chloroform 10:90)].
WORKUP
后处理
- temperaturerefluxed for 1 h
- customabsorbed directly on silicagel (10 g)