반응 #1563

반응 방정식

water

glycine ethyl ester hydrochloride

4-fluoro-3-nitrophenyl isocyanate

triethylamine

→

title product

수율 56.1%

N-[(4-Fluoro-3-nitrophenyl)carbamoyl]glycine, ethyl ester

수율 56.1%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도while maintaining the temperature below 10° C.
2. 2
   추출The aqueous mixture is extracted with ether
3. 3
   세척The combined organic extracts are washed sequentially with 1N hydrochloric acid and brine
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   농축concentrated in vacuo
6. 6
   기타to obtain a solid which
7. 7
   기타is air-dried

실험 절차

A solution of 4-fluoro-3-nitrophenyl isocyanate (10 g, 0.055 mol) in anhydrous tetrahydrofuran is cooled to 0° C., treated with glycine ethyl ester hydrochloride (7.7 g, 0.055 mol), treated with triethylamine (5.56 g, 0.055 mol) while maintaining the temperature below 10° C., stirred at room temperature for 1 hour and poured into water. The aqueous mixture is extracted with ether. The combined organic extracts are washed sequentially with 1N hydrochloric acid and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain a solid which is air-dried to give the title product as a yellow solid (8.8 g, mp 115°-120° C.).

출처