反应 #157480

反应方程式

4-(3-bromophenyl)-2,4-dihydro-3H-1,2,4-triazol-3-one

NaH

1,1′,1″-(chloromethanetriyl)tribenzene

→

4-(3-bromophenyl)-2-(triphenylmethyl)-2,4-dihydro-3H-1,2,4-triazol-3-one

溶剂

DMF

EtOAc

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture stirred at room temperature for 4 hr
2. 2
   洗涤washed with H2O and brine
3. 3
   干燥dried over Na2SO4
4. 4
   浓缩then concentrated in vacu
5. 5
   其他The residue was purified by silica gel chromatography (EtOAc/Hexanes)

实验过程

A mixture of 4-(3-bromophenyl)-2,4-dihydro-3H-1,2,4-triazol-3-one (250 mg, 1.04 mmol) and NaH (50 mg of a 60% dispersion in mineral oil, 1.25 mmol) in DMF (3 mL) was stirred at room temperature for 30 min. To the solution was added 1,1′,1″-(chloromethanetriyl)tribenzene (305 mg, 1.09 mmol) and the mixture stirred at room temperature for 4 hr. The reaction mixture was diluted with EtOAc, washed with H2O and brine, dried over Na2SO4 then concentrated in vacu. The residue was purified by silica gel chromatography (EtOAc/Hexanes) to give 4-(3-bromophenyl)-2-(triphenylmethyl)-2,4-dihydro-3H-1,2,4-triazol-3-one as a pale yellow foam. 1H NMR (400 MHz, DMSO-d6) δ 7.22-7.31 (m, 15 H), 7.40-7.42 (m, 1H), 7.51 (d, J=7.8 Hz, 1H), 7.63 (d, J=7.8 Hz, 1H), 7.90 (s, 1H), 8.60 (s, 1H).

来源