反応 #440254

反応方程式

pyrazole

4-(3,5-Dichlorobenzyl)-3,5-dimethyl-1H-pyrazole

2-chloroethylamine hydrochloride

→

title compound

収率 19.3%

2-[4-(3,5-Dichlorobenzyl)-3,5-dimethyl-1H-pyrazol-1-yl]ethanamine

収率 19.3%

溶媒

dichloromethane

toluene

反応条件

後処理

1. 1
   温度After cooling
2. 2
   洗浄washed with 2 M aqueous sodium hydroxide solution (20 ml)
3. 3
   乾燥dried over anhydrous magnesium sulphate
4. 4
   ろ過filtered
5. 5
   濃縮concentrated under reduced pressure
6. 6
   その他The crude product was purified by flash chromatography on silica gel eluting with methanol:dichloromethane:ammonia (5:95:0.5, by volume)

実験手順

A stirred suspension of the pyrazole (200 mg, 0.78 mmol) of Example 23 and 2-chloroethylamine hydrochloride (136 mg, 1.18 mmol) in toluene (1 ml) was heated at 120° C. in a sealed Reacti-vial (Trade Mark) for 18 hours. After cooling, the mixture was diluted with dichloromethane (30 ml), washed with 2 M aqueous sodium hydroxide solution (20 ml), dried over anhydrous magnesium sulphate, filtered and concentrated under reduced pressure. The crude product was purified by flash chromatography on silica gel eluting with methanol:dichloromethane:ammonia (5:95:0.5, by volume) to afford the title compound (45 mg) as white crystals, m.p. 70-72° C.

出典