반응 #53315

반응 방정식

hydrochloric acid

Glycine ethyl ester hydrochloride

triethylamine

6-chloronaphthalene-2-sulfonyl chloride

→

title compound

수율 101.4%

ethyl 2-[(6-chloronaphthalen-2-ylsulfonyl)amino]acetate

수율 101.4%

용매

methylene chloride

반응 조건

후처리

1. 1
   온도under cooling with ice
2. 2
   추출the mixture was extracted with methylene chloride
3. 3
   세척The methylene chloride layer was washed with saturated sodium chloride solution
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
6. 6
   세척After washing the resulting crystals in n-hexane
7. 7
   여과the crystals were collected by filtration
8. 8
   기타air-dried

실험 절차

Glycine ethyl ester hydrochloride (9.88 g) was suspended in methylene chloride (500 ml), and triethylamine (20.2 ml) and then 6-chloronaphthalene-2-sulfonyl chloride (17.6 g) were added to the suspension under cooling with ice. After stirring at room temperature for 1 hour and adjusting the mixture to pH 2 by addition of 1N hydrochloric acid, the mixture was extracted with methylene chloride. The methylene chloride layer was washed with saturated sodium chloride solution and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. After washing the resulting crystals in n-hexane, the crystals were collected by filtration and air-dried to obtain the title compound (22.4 g).

출처