HRID1274692

反应详情

EQUATION

反应方程式

HRID 1274692 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 8 ml of acetic acid were added 1.00 g of 2-benzylamino-4-(t-butylamino)-5-fluoropyrimidine together with 215 mg of 10% palladium on carbon, and the mixture was hydrogenated at 60° C. for ten days. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. The procedure of adding 10 ml of ethanol and concentrating under reduced pressure was repeated three times, and the residue was separated by column chromatography (silica gel, 25 g; eluent: chloroform, and then, chloroform:methanol, 200:1), and the corresponding fractions were collected and concentrated under reduced pressure to obtain 360 mg of the title compound as a pale gray solid.

WORKUP

后处理

  1. waitthe mixture was hydrogenated at 60° C. for ten days
  2. customThe catalyst was separated by filtration
  3. distillationthe solvent and the like were distilled off under reduced pressure
  4. additionThe procedure of adding 10 ml of ethanol
  5. concentrationconcentrating under reduced pressure
  6. customthe residue was separated by column chromatography (silica gel, 25 g
  7. customeluent: chloroform, and then, chloroform:methanol, 200:1), and the corresponding fractions were collected
  8. concentrationconcentrated under reduced pressure