反応 #531850

反応方程式

1-(3-chlorophenyl)piperazine hydrochloride

triethylamine

ethyl 6-bromohexanoate

→

ethyl 6-[N′-(3-chlorophenyl)-N-piperazinyl]hexanoate

収率 59.6%

溶媒

toluene

反応条件

後処理

1. 1
   温度the mixture heated
2. 2
   温度at reflux for 4 hours
3. 3
   洗浄washed with water (2×100 ml), brine (100 ml)
4. 4
   乾燥dried over Na2SO4
5. 5
   ろ過filtered
6. 6
   濃縮concentrated to dryness
7. 7
   その他The residue obtained
8. 8
   その他was purified by flash chromatography on silica gel

実験手順

To a solution of 1-(3-chlorophenyl)piperazine hydrochloride (12 g, 0.051 mol) in anhydrous toluene (250 ml) was added triethylamine (TEA) (15.6 ml, 0.112 mol) and ethyl 6-bromohexanoate (13.6 g, 0.061 mol) and the mixture heated at reflux for 4 hours. The mixture was then cooled to room temperature, washed with water (2×100 ml), brine (100 ml), dried over Na2SO4, filtered and concentrated to dryness. The residue obtained was purified by flash chromatography on silica gel using ethyl acetate/hexane (1/1) to give ethyl 6-[N′-(3-chlorophenyl)-N-piperazinyl]hexanoate (10.3 g) as a clear oil.

出典