HRID583675

反应详情

EQUATION

反应方程式

HRID 583675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Pyrimidine 19-8 (1.05 g, 1.75 mmol) was dissolved in a mixture of acetic acid (50 mL) and conc HCl (4.5 mL). After addition of 10% Pd/C (450 mg) the mixture was shaken on a Parr hydrogenator under 45 psi H2 pressure for 2 h. The reaction mixture was filtered, concentrated, azeotroped with toluene, and purified by flash chromatography (silica 20:1:1 then 8:1:1 EtOH/NH4OH/H2O) providing 19-9 as a white solid.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. concentrationconcentrated
  3. customazeotroped with toluene
  4. custompurified by flash chromatography (silica 20:1:1