HRID1772893

反应详情

EQUATION

反应方程式

HRID 1772893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

10% Pd/C (1 g) was added to a solution of tert-butyl(2-methoxy-5-nitropyridin-3-yl)methylcarbamate (9.8 g, 34.6 mmol) in MeOH (150 mL) and DCM (75 mL) and the mixture stirred at rt for 7 h under an atmosphere of H2. The reaction mixture was then filtered through celite and washed with MeOH and the filtrate concentrated in vacuo. Purification by flash column chromatography eluting with 2:1 to 1:1 heptane-EtOAc yielded the title compound (7.4 g, 29.2 mmol) as a tan solid.

WORKUP

后处理

  1. filtrationThe reaction mixture was then filtered through celite
  2. washwashed with MeOH
  3. concentrationthe filtrate concentrated in vacuo
  4. customPurification by flash column chromatography
  5. washeluting with 2:1 to 1:1 heptane-EtOAc