反応 #1591407

反応方程式

Potassium carbonate

sodium iodide

2-phenyl piperidine

7-(3-chloropropoxy)-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

Hydrogen chloride ethyl acetate

→

title compound

収率 27.7%

1-ethyl-3,3,5-trimethyl-7-[3-(2-phenylpiperidin-1-yl)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione hydrochloride

収率 27.7%

溶媒

Water

DMF

ethyl acetate

反応条件

後処理

1. 1
   温度The reaction mixture was cooled to room temperature
2. 2
   抽出followed by extraction by ethyl acetate
3. 3
   洗浄The organic layer was washed with water
4. 4
   乾燥with saturated saline, and dried with anhydrous magnesium sulfate
5. 5
   その他After condensation under reduced pressure
6. 6
   その他the residue was purified by silica gel column chromatography (hexane: ethyl acetate=2:1→1:1)
7. 7
   その他condensed under reduced pressure
8. 8
   workup.STIRRINGwas stirred at room temperature
9. 9
   その他condensed to dryness under reduced pressure

実験手順

Potassium carbonate(0.54 g), sodium iodide(0.21 g), and 2-phenyl piperidine(0.23 g) were added to a DMF solution(15 ml) of 7-(3-chloropropoxy)-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione(0.44 g). The mixture was stirred at 70° C. for 5 hours. The reaction mixture was cooled to room temperature. Water was added thereto, followed by extraction by ethyl acetate. The organic layer was washed with water and then with saturated saline, and dried with anhydrous magnesium sulfate. After condensation under reduced pressure, the residue was purified by silica gel column chromatography (hexane: ethyl acetate=2:1→1:1). The purified product was condensed under reduced pressure. A 4N-Hydrogen chloride ethyl acetate solution(0.2 ml) was added to an ethyl acetate solution (10 ml) of the residue, which was stirred at room temperature. The liquid was condensed to dryness under reduced pressure to give the title compound(0.18 g) as a white amorphous solid.

出典