HRID2071018

反应详情

EQUATION

反应方程式

HRID 2071018 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10% Pd/C (0.010 g) was added to a stirred solution of 2-amino-6-methoxypyrimidine-4-carbonitrile (0.107 g, 0.71 mmol, 1 eq) in 4 ml HOAc. A H2 balloon (20 psi) was added. After 2 h the mixture was filtered through Celite. The filter cake was rinsed with MeOH. The organics were combined and the solvent was removed in vacuo. 1 N NaOH was added to pH>8 and the solvent was removed in vacuo. The residue was stirred in EtOAc (30 ml) and saturated aqueous NaHCO3 (1 ml). After 30 min Na2SO4 was added and the mixture was stirred for 10 min. The inorganics were filtered off, and the solvent was removed in vacuo yielding 0.1044 g (0.68 mmol, 95% yield) of the product.

WORKUP

后处理

  1. additionA H2 balloon (20 psi) was added
  2. filtrationAfter 2 h the mixture was filtered through Celite
  3. washThe filter cake was rinsed with MeOH
  4. customthe solvent was removed in vacuo
  5. addition1 N NaOH was added to pH>8
  6. customthe solvent was removed in vacuo
  7. additionAfter 30 min Na2SO4 was added
  8. stirringthe mixture was stirred for 10 min
  9. filtrationThe inorganics were filtered off
  10. customthe solvent was removed in vacuo