HRID1269134

反应详情

EQUATION

反应方程式

HRID 1269134 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3.10 g of tert-butyl 4-(3-aminophenyl)-3,6-dihydro-1(2H)-pyridinecarboxylate (11.3 mmol) and 1.0 g of 10% Pd/C in 200 mL of ethanol was hydrogenated at room temperature using the balloon method for 2 days. The reaction mixture was filtered through Celite and washed with ethanol. The combined ethanol extracts were concentrated in vacuo and the residue was chromatographed on silica (dichloromethane:methanol:isopropylamine=95:5:1) to give 2.63 g of the desired product (84%): ESMS m/e: 277.2 (M+H)+.

WORKUP

后处理

  1. customwas hydrogenated at room temperature
  2. customfor 2 days
  3. filtrationThe reaction mixture was filtered through Celite
  4. washwashed with ethanol
  5. concentrationThe combined ethanol extracts were concentrated in vacuo
  6. customthe residue was chromatographed on silica (dichloromethane:methanol:isopropylamine=95:5:1)