HRID68961

反应详情

EQUATION

反应方程式

HRID 68961 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customwas carried out at room temperature under 4 atm
  2. customThe catalyst was removed by celite filtration
  3. concentrationfollowed by concentration under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate:methanol=9:1→5:5)
  5. customcondensed under reduced pressure