HRID1038732

反应详情

EQUATION

反应方程式

HRID 1038732 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of tert-butyl {6-[3-(2-methyl-5-nitro-phenyl)-1-methyl-ureido]-pyrimidin-4-yl}-carbamate (330 mg, 0.82 mmol) in a mixture of methanol (20 ml) and DMF (50 ml) is hydrogenated in the presence of 10% palladium on charcoal (500 mg) at atmospheric pressure. After 20 h the hydrogenation is complete and the catalyst is filtered off. The filtrate is evaporated to dryness. The residue obtained is triturated with ether, filtered off, and vacuum dried to afford a gray powder: HPLC: tR=5.38 min (purity: 97%, gradient A), ESI-MS: 373.4 [MH]+.

WORKUP

后处理

  1. filtrationthe catalyst is filtered off
  2. customThe filtrate is evaporated to dryness
  3. customThe residue obtained
  4. customis triturated with ether
  5. filtrationfiltered off
  6. customvacuum dried
  7. customto afford a gray powder