HRID2407674

反应详情

EQUATION

反应方程式

HRID 2407674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of the compound prepared in Example 59 (100 mg) and 4,6-diamino-2-ethoxynicotinonitrile (50 mg, prepared according to the preparation reported in Szczepankiewicz, B. G.; et al. J. Med. Chem. 2006, 49, 3563 and references therein) in pyridine (1.5 mL) was heated to 50° C. overnight and then 80° C. for six days. The mixture was cooled to room temperature, diluted with ethyl acetate and washed twice with a saturated aqueous sodium bicarbonate solution. The organic phase was dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (ethyl acetate:hexane=4:1) to obtain the title compound (18 mg) having the following physical data.

WORKUP

后处理

  1. customprepared
  2. washwashed twice with a saturated aqueous sodium bicarbonate solution
  3. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography on silica gel (ethyl acetate:hexane=4:1)