HRID2351085

反应详情

EQUATION

反应方程式

HRID 2351085 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 1.71 g. (ca. 5 mmol) crude 1,4-dihydro-4-oxo-5-(phenylmethoxy)-N-(tetrahydro-2-oxo-1(2H)-pyrimidinyl)-2-pyridine-carboxamide in 22 ml acetonitrile was added 4.1 g (20 mmol) bis(trimethylsilyl)acetamide. After stirring for 20 minutes the undissolved dicyclohexylurea was filtered off and 0.85 g palladium on carbon were added to the filtrate. After the mixture had been hydrogenated for one hour, the catalyst was removed by filtration and 2.1 ml methanol and 0.1 ml acetic acid were added to the filtrate. After stirring overnight the desired product was filtered off and dried in vacuo. Yield 0.7 g, melting point 285°-290° C. (dec.).

WORKUP

后处理

  1. additionTo a suspension of 1.71 g
  2. filtrationwas filtered off
  3. addition0.85 g palladium on carbon were added to the filtrate
  4. customthe catalyst was removed by filtration and 2.1 ml methanol and 0.1 ml acetic acid
  5. additionwere added to the filtrate
  6. filtrationwas filtered off
  7. customdried in vacuo