HRID1504134
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
10% Palladium on carbon(0.3 g) was added to an acetic acid solution (20 ml) of 1-ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-carbonitrile(1.4 g), and catalytic reduction was carried out at room temperature under 4 atm. The catalyst was removed by celite filtration, followed by concentration under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate: methanol=9:1→5:5). The purified product was condensed under reduced pressure to give the title compound(0.19 g) as a colorless oily matter.
WORKUP
后处理
- customwas carried out at room temperature under 4 atm
- customThe catalyst was removed by celite filtration
- concentrationfollowed by concentration under reduced pressure
- customThe residue was purified by silica gel column chromatography (ethyl acetate: methanol=9:1→5:5)
- customcondensed under reduced pressure