HRID1957986

反应详情

EQUATION

反应方程式

HRID 1957986 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of [(2-chloro-5-nitro-pyrimidin-4-yl)-isopropyl-amino]-acetic acid ethyl ester (40 g; 0.132 mol), Pt/C5% (2 g) and vanadylacetylacetonate (2 g; 0.754 mmol) in THF (50 ml) was treated with hydrogen (5 bar) overnight. The reaction mixture was warmed (in order to solubilize the precipitate formed) and filtered on a celite pad, then concentrated in vacuo. The crude was diluted in ethyl acetate and the organic phase was washed with NaOH 10% solution, dried with MgSO4 and concentrated in vacuo. 28 g (0.115 mol; 87% yield) of solid material were obtained.

WORKUP

后处理

  1. temperatureThe reaction mixture was warmed (in order
  2. customformed) and
  3. filtrationfiltered on a celite pad
  4. concentrationconcentrated in vacuo
  5. additionThe crude was diluted in ethyl acetate
  6. washthe organic phase was washed with NaOH 10% solution
  7. dry with materialdried with MgSO4
  8. concentrationconcentrated in vacuo
  9. custom28 g (0.115 mol; 87% yield) of solid material were obtained