HRID1695097

反应详情

EQUATION

反应方程式

HRID 1695097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,6-Diamino-5-nitroso-4-[4-(2,2,2-trifluoro-acetylamino-methyl)-benzyloxy]-pyrimidine (1.22 g, 3.3 mmol) and triphenylphosphine (1.89 g, 7 mmol) in 20 mL o-xylene are heated to reflux for 1 h. After cooling to room temperature the solvent is removed in vacuo and the remaining residue redissolved in methanol. The residue is adsorbed on SiO2 and purified by flash column chromatography (CH2Cl2/methanol 95:5 to 5:1) to yield the title compound.

WORKUP

后处理

  1. temperatureto reflux for 1 h
  2. customis removed in vacuo
  3. dissolutionthe remaining residue redissolved in methanol
  4. custompurified by flash column chromatography (CH2Cl2/methanol 95:5 to 5:1)