反応 #66513

ord-aefa367428334f35889df964d4cf7e2b

反応方程式

Ic1cn[nH]c1
4-iodo-1H-pyrazole
COc1ccc(CCl)cc1
1-(chloromethyl)-4-methoxybenzene
O=C([O-])[O-].[K+].[K+]
K2CO3
COc1ccc(Cn2cc(I)cn2)cc1
4-iodo-1-(4-methoxybenzyl)-1H-pyrazole
収率 88.2%

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture was cooled to room temperature
  2. 2
    ろ過was filtered
  3. 3
    濃縮The filtrate was concentrated under reduced pressure
  4. 4
    その他The crude product was purified by flash chromatography over silica gel

実験手順

According to Scheme 6 Step 1: A suspension of 4-iodo-1H-pyrazole (26.3 mmol, 5.11 g), 1-(chloromethyl)-4-methoxybenzene (29.0 mmol, 3.95 mL) and K2CO3 (39.5 mmol, 5.46 g) in acetonitrile (150 mL) was heated at 60° C. overnight. The reaction mixture was cooled to room temperature and was filtered. The filtrate was concentrated under reduced pressure. The crude product was purified by flash chromatography over silica gel using DCM as eluent to afford 4-iodo-1-(4-methoxybenzyl)-1H-pyrazole (23.2 mmol, 7.3 g, 88%) as a yellow solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08524718B2uspto-grants-2013_09