HRID1788068

反应详情

EQUATION

反应方程式

HRID 1788068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of intermediate 17 (0.0006 mol) in toluene (10 ml) was stirred and refluxed for 5 hours, then brought to room temperature and the solvent, was evaporated till dryness. The residue was taken up in DCM. The solvent was evaporated till dryness. The residue was purified by column chromatography over kromasil® (10 μm) (eluent: DCM/MeOH/Et3N 95/5/0.5). The pure fractions were collected and the solvent was evaporated. The residue (0.12 g, 40%) was taken up in DCM. The solvent was evaporated till dryness, yielding 0.08 g (27%) of 9-(3-chlorophenyl)-4,9-dihydro-α-(4-methoxyphenyl)-α-(1-methyl-1H-imidazol-5-yl)-tetrazolo[5,1-b]quinazoline-7-methanol (compound 3).

WORKUP

后处理

  1. temperaturerefluxed for 5 hours
  2. custombrought to room temperature
  3. customthe solvent, was evaporated till dryness
  4. customThe solvent was evaporated till dryness
  5. customThe residue was purified by column chromatography over kromasil® (10 μm) (eluent: DCM/MeOH/Et3N 95/5/0.5)
  6. customThe pure fractions were collected
  7. customthe solvent was evaporated
  8. customThe solvent was evaporated till dryness