HRID81908

反应详情

EQUATION

反应方程式

HRID 81908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A Parr vessel was charged with 10% Pd/C (0.6 g) and a suspension of 1-[4-amino-7-bromo-2-(2-methoxyethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]-2-methylpropan-2-ol (4.0 g) in acetonitrile (150 mL) and methanol (50 mL). The vessel was placed under hydrogen pressure (50 psi, 3.4×105 Pa) for 3 hours. The reaction mixture was diluted with 1/1 chloroform/methanol (100 mL), filtered through a layer of CELITE filter aid, and concentrated under reduced pressure. The residue was triturated with acetonitrile to provide 3.55 g of 1-[4-amino-2-(2-methoxyethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]-2-methylpropan-2-ol hydrobromide as a white powder, mp 234-235° C. Anal. calcd for C16H22BrN5O2: % C, 48.49; % H, 5.60; % N, 17.67. Found: % C, 48.64; % H, 5.69; % N, 17.62.

WORKUP

后处理

  1. customfor 3 hours
  2. filtrationfiltered through a layer of CELITE
  3. filtrationfilter aid
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was triturated with acetonitrile