HRID2085403

反应详情

EQUATION

反应方程式

HRID 2085403 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)-1,2,3,6-tetrahydropyridine-1-carboxylate (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 and washed with ethanol. The combined ethanol extracts were concentrated in vacuo and the residue was chromatographed on silica (dichloromethane: methanol 95:5 with 1% isopropylamine added to protect the BOC group from hydrolysis) to give 2.63 g of the desired product (84%).

WORKUP

后处理

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