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
A solution of 1,1-dimethylethyl 4-[4-(ethoxycarbonyl)-2-thiazolyl]-1-piperidinecarboxylate (11.1 g, 32.7 mmol) (i.e. the product of Example 1, Step A) in diethyl ether (100 mL) at 0° C. was treated with a solution of hydrogen chloride in diethyl ether (2 M, 166 mL, 331 mmol). The reaction mixture then was diluted with absolute ethanol (100 mL) and stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure, re-dissolved in ethanol and evaporated again to leave a solid. The resulting solid was placed under a high vacuum for several hours to give 10.38 g of the title compound as a hygroscopic white powder. This compound was of sufficient purity to use in subsequent reactions.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- dissolutionre-dissolved in ethanol
- customevaporated again
- customto leave a solid
- waitThe resulting solid was placed under a high vacuum for several hours