HRID2351085
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionTo a suspension of 1.71 g
- filtrationwas filtered off
- addition0.85 g palladium on carbon were added to the filtrate
- customthe catalyst was removed by filtration and 2.1 ml methanol and 0.1 ml acetic acid
- additionwere added to the filtrate
- filtrationwas filtered off
- customdried in vacuo