反応 #82237

反応方程式

ethylenediamine

hydrochloric acid

ethanol

ethanol

ethyl 2-ethoxycarbonyl-2-[4-(2-ethoxy-2-iminoethoxy]phenyl]acetate

ethanol

→

title compound

収率 54.8%

ethyl 2-ethoxycarbonyl-2-[4-[(2-imidazolin-2-yl)methoxy]phenyl]acetate

収率 54.8%

溶媒

water

反応条件

後処理

1. 1
   その他obtained in the above step b)
2. 2
   workup.STIRRINGthe resulting mixture was stirred at room temperature for 1.5 hours
3. 3
   温度by refluxing
4. 4
   温度under heating for 0.5 hours
5. 5
   温度After cooling
6. 6
   その他the resulting reaction solution
7. 7
   濃縮concentrated to dryness
8. 8
   その他The residue thus obtained
9. 9
   洗浄washed with diethyl ether
10. 10
    その他thus precipitated
11. 11
    ろ過were collected by filtration

実験手順

With ice cooling and stirring, 40 ml of ethanol solution containing 3.6 g of ethyl 2-ethoxycarbonyl-2-[4-(2-ethoxy-2-iminoethoxy]phenyl]acetate obtained in the above step b) was added dropwise to a 10 ml ethanol solution containing 0.6 g of ethylenediamine, and the resulting mixture was stirred at room temperature for 1.5 hours, followed by refluxing under heating for 0.5 hours. After cooling, the resulting reaction solution was adjusted to an acidic pH with ethanol containing 13% (w/v) of hydrochloric acid, and then concentrated to dryness. The residue thus obtained was dissolved in water and washed with diethyl ether. Thereafter, the resulting water layer was adjusted to pH 9-10 with dilute sodium hydroxide aqueous solution, and crystals thus precipitated were collected by filtration. In this way, 1.83 g of the title compound was obtained in the form of colorless crystals.

出典