HRID2407659

反应详情

EQUATION

反应方程式

HRID 2407659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of the compound prepared in Example 7 (2.00 g), tert-butyl piperidin-4-ylmethylcarbamate (2.72 g) and acetic acid (0.66 mL) in acetonitrile (60 mL) was stirred at room temperature for 30 minutes. Tetramethylammonium triacetoxyborohydride (9.12 g) was added and the reaction was stirred overnight. The reaction was then poured into a saturated aqueous sodium bicarbonate solution and the resulting mixture was extracted three times with ethyl acetate. The combined organics were dried with anhydrous magnesium sulfate and concentrated to a white solid. The solid was triturated with hexane to obtain the title compound (3.90 g) having the following physical data.

WORKUP

后处理

  1. extractionthe resulting mixture was extracted three times with ethyl acetate
  2. dry with materialThe combined organics were dried with anhydrous magnesium sulfate
  3. concentrationconcentrated to a white solid
  4. customThe solid was triturated with hexane