HRID81907

反应详情

EQUATION

反应方程式

HRID 81907 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-{7-bromo-4-[(2-hydroxy-2-methylpropyl)amino][1,5]naphthyridin-3-yl}-3-methoxypropionamide hydrochloride (60.00 g, 138 mmol), potassium carbonate (60 g), water (300 mL), and ethanol (900 mL) was heated at reflux for 16 hours and then concentrated under reduced pressure. The precipitated solid was isolated by filtration, washed sequentially with water and methanol, and dried to provide a brown solid. This material was dissolved in a 3/1 mixture of chloroform/methanol and decolorized with activated charcoal to provide 38.5 g of 1-[7-bromo-2-(2-methoxyethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]-2-methylpropan-2-ol as a white solid, mp 125° C. Anal. calcd for C16H19BrN4O2: % C, 50.67; % H, 5.05; % N, 14.77. Found: % C, 50.86; % H, 4.94; % N, 15.01.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 16 hours
  3. concentrationconcentrated under reduced pressure
  4. customThe precipitated solid was isolated by filtration
  5. washwashed sequentially with water and methanol
  6. customdried
  7. customto provide a brown solid