HRID2257016

反应详情

EQUATION

反应方程式

HRID 2257016 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To an ice-cooled solution of 1-cyclopentyl-3-phenylmethyl-4-cyano-5-(phenylmethylcarbonylamino)-1H-pyrazole (1.1 g, 2.8 mmol) in ethanol (30 ml) was added 30% H2O2 (2.5 ml), followed by NaOH (100 mg) dissolved in water (5 ml). The reaction mixture was stirred a such for 1 hour, then at room temperature for 1 hour, then it was heated on a steam bath for 3.5 hours and finally it was stirred at room temperature overnight. The reaction mixture was concentrated to dryness, and partitioned between water (25 ml) and CHCl3 (50 ml). The organic layer was separated, and concentrated in vacuo and the oily residue was crystallized from isopropanol to afford 234 mg (22%) of 1-cyclopentyl-3-phenylmethyl-6-(phenylmethyl)-pyrazolo[3,4-d]pyrimidin-4-one, as a white solid, m.p. 204°-206° C.

WORKUP

后处理

  1. waitat room temperature for 1 hour
  2. temperatureit was heated on a steam bath for 3.5 hours
  3. stirringfinally it was stirred at room temperature overnight
  4. concentrationThe reaction mixture was concentrated to dryness
  5. custompartitioned between water (25 ml) and CHCl3 (50 ml)
  6. customThe organic layer was separated
  7. concentrationconcentrated in vacuo
  8. customthe oily residue was crystallized from isopropanol