反应详情

A 60˜70% aqueous solution of ethylamine (3.6 mL) and a 20% aqueous NaOH solution (8.0 mL) were added dropwise respectively into a solution of 2-chloro-5-chloromethylthiazole (3.40 g) in chloroform (40 mL), then benzyl triethyl ammonium chloride (0.1 g) was added. After stirring overnight at room temperature, the pH of the resulting mixture was adjusted to weak alkaline. The organic layer was separated while the aqueous layer was extracted with dichloromethane twice. The organic phases were combined, and dried over anhydrous sodium sulfate after washed with an iced aqueous sodium chloride solution twice, then remove the solvent under reduced pressure to obtain 2-chloro-5-ethylaminomethylthiazole 3.37 g as an oil in 95.2% purity. GC-MS: (M+) (EI, 70 eV, m/z) calc: 176. found: 176.

1. customThe organic layer was separated while the aqueous layer
2. extractionwas extracted with dichloromethane twice
3. dry with materialdried over anhydrous sodium sulfate
4. washafter washed with an iced aqueous sodium chloride solution twice
5. customremove the solvent under reduced pressure