HRID1957986
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
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
- temperatureThe reaction mixture was warmed (in order
- customformed) and
- filtrationfiltered on a celite pad
- concentrationconcentrated in vacuo
- additionThe crude was diluted in ethyl acetate
- washthe organic phase was washed with NaOH 10% solution
- dry with materialdried with MgSO4
- concentrationconcentrated in vacuo
- custom28 g (0.115 mol; 87% yield) of solid material were obtained