反応 #61070

反応方程式

water CH2Cl2

3-bromo-pyrazole

triphenylmethyl chloride

Et3N

→

title compound

収率 64.0%

3-Bromo-1-(triphenylmethyl)-1H-pyrazole

収率 64.0%

溶媒

CH2Cl2

反応条件

後処理

1. 1
   その他The phases were separated
2. 2
   抽出the aqueous layer was further extracted with CH2Cl2 (2×30 mL)
3. 3
   乾燥The combined organic extracts were dried over anh. Na2SO4
4. 4
   ろ過the solids were filtered
5. 5
   その他the solvent evaporated
6. 6
   その他The residue was purified by flash chromatography (silica gel, 100% CH2Cl2)

実験手順

To a solution of 3-bromo-pyrazole (2.0 g, 13.6 mmol) in anh. CH2Cl2 (40 mL), at r.t., under N2, were added triphenylmethyl chloride (4.17 g, 1.1 eq) and Et3N (2.1 mL, 1.1 eq). The reaction mixture was stirred at r.t. for 4 hr. It was poured into water/CH2Cl2. The phases were separated and the aqueous layer was further extracted with CH2Cl2 (2×30 mL). The combined organic extracts were dried over anh. Na2SO4, the solids were filtered and the solvent evaporated. The residue was purified by flash chromatography (silica gel, 100% CH2Cl2) to give the title compound as a white solid (3.39 g, 64%).

出典