HRID1252594

反应详情

EQUATION

反应方程式

HRID 1252594 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 12 g (0.0365 mol) of 1,4-dihydro-4-oxo-N-(2-oxo-1-imidazolidinyl)-5-(phenylmethoxy)-2-pyridinecarboxamide in 150 ml of acetonitrile was added 36.1 ml (0.146 mol) of bis(trimethylsilyl)acetamide to form a slightly turbid solution. After filtration, 6 g of 10% palladium on charcoal was added and hydrogen was passed through the stirred reaction mixture. After hydrogenation for 60 minutes, the catalyst was filtered off and 15 ml of methanol and 2 ml of acetic acid were added. Stirring was continued overnight; the title compound crystallized out, yielding 6.6 g, melting point 270°-275° C.

WORKUP

后处理

  1. customto form a slightly turbid solution
  2. filtrationAfter filtration, 6 g of 10% palladium on charcoal
  3. additionwas added
  4. customhydrogen was passed through the stirred reaction mixture
  5. filtrationthe catalyst was filtered off
  6. addition15 ml of methanol and 2 ml of acetic acid were added
  7. waitwas continued overnight
  8. customthe title compound crystallized out
  9. customyielding 6.6 g, melting point 270°-275° C.