HRID1920045

反应详情

EQUATION

反应方程式

HRID 1920045 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In an autoclave, 5 g 6-chloro-N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2-pyrimidine amine, 0.5 g palladium on charcoal 5% wet with 50% water, 50 mL ethanol and 5 mL triethylamine is charged. The mixture is hydrogenated at 5 bars and room temperature for 40 hours. Once completed the conversion, the catalyst is filtered off and the filtrates is concentrated in vacuum. The residue is taken again with isopropyl acetate and an aqueous carbonate solution. The layers are separated, and the organic layer is concentrated, yielding, upon drying, 3 g of product with 85% HPLC purity (A %), which is identified through LC-MS and 1H-NMR.

WORKUP

后处理

  1. filtrationthe catalyst is filtered off
  2. concentrationthe filtrates is concentrated in vacuum
  3. customThe layers are separated
  4. concentrationthe organic layer is concentrated
  5. customyielding
  6. customupon drying