HRID660040

反应详情

EQUATION

反应方程式

HRID 660040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionre-dissolved in ethanol
  3. customevaporated again
  4. customto leave a solid
  5. waitThe resulting solid was placed under a high vacuum for several hours