HRID1029401

反应详情

EQUATION

反应方程式

HRID 1029401 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of ethyl 5-tert-butyl-4,5-dihydro-4-oxo-imidazo[1,5-a]quinoxaline-3-carboxylate (1.6 g, 5 mmol) and pinacolone (1.25 ml, 10 mmol) in dry tetrahydrofuran (THF) (30 ml) was added sodium hydride (200 mg, 80% in mineral oil, 6.9 mmol). The mixture was brought to reflux for 2 h, then cooled to room temperature and neutralized with acetic acid. After evaporation of the solvent the residue was partitioned between sat. aqueous NaHCO3 (10 ml) and methylene chloride (30 ml). The organic phase was dried over Na2SO4 and evaporated to give the title compound as yellow crystals. M.p. 190°-191 ° C. (Compound 1).

WORKUP

后处理

  1. temperatureto reflux for 2 h
  2. customAfter evaporation of the solvent the residue
  3. customwas partitioned between sat. aqueous NaHCO3 (10 ml) and methylene chloride (30 ml)
  4. dry with materialThe organic phase was dried over Na2SO4
  5. customevaporated