HRID1743816

反应详情

EQUATION

反应方程式

HRID 1743816 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of tert-butyl 4-[(dibenzylamino)carbonyl]piperidine-1-carboxylate (EXAMPLE 4, Step 1, 4.0 g, 10.0 mmol) in methanol (550 mL) was added 4N HCl dioxane solution (80 mL, 320 mmol) at 0° C. The mixture was stirred for 6 h and evaporated. The resulting amorphous was dissolved in aqueous ammonia and the mixture was extracted with dichloromethane. The combined extract was dried over magnesium sulfate, and concentrated to afford 3.0 g (99%) of the title compound as a colorless amorphous powder.

WORKUP

后处理

  1. customevaporated
  2. dissolutionThe resulting amorphous was dissolved in aqueous ammonia
  3. extractionthe mixture was extracted with dichloromethane
  4. extractionThe combined extract
  5. dry with materialwas dried over magnesium sulfate
  6. concentrationconcentrated