HRID423195

反应详情

EQUATION

反应方程式

HRID 423195 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 5-(4-bromophenyl)-3-t-butyl-4-(2-methoxyphenyl)-4,5-dihydro-1H-pyrrolo[3,4-c]pyrazol-6-one (0.10 g, 0.23 mmol), 3-furylboronic acid (0.038 g, 0.34 mmol), tripotassium phosphate (0.096 g, 0.45 mmol) and butanol (1 mL), (2′,4′,6′-tri-isopropylbiphenyl-2-yl)phosphine (0.009 g, 0.02 mmol) and tris(dibenzylideneacetone)dipalladium(0) (0.004 g, 0.004 mmol) were added under a nitrogen atmosphere, and the mixture was stirred under reflux for 3 hr. The reaction mixture was purified by silica gel column chromatography (ethyl acetate/n-hexane). The fraction was concentrated under reduced pressure and the precipitate was collected by filtration to give 3-t-butyl-5-(4-fur-3-ylphenyl)-4-(2-methoxyphenyl)-4,5-dihydro-1H-pyrrolo[3,4-c]pyrazol-6-one (0.061 g, 63%) as colorless crystals.

WORKUP

后处理

  1. additionwere added under a nitrogen atmosphere
  2. temperatureunder reflux for 3 hr
  3. customThe reaction mixture was purified by silica gel column chromatography (ethyl acetate/n-hexane)
  4. concentrationThe fraction was concentrated under reduced pressure
  5. filtrationthe precipitate was collected by filtration