반응 #1328393

반응 방정식

benzyl chloroformate

3-aminopropanol

→

title compound

수율 58.9%

N-CBZ-3-aminopropanol

수율 58.9%

용매

CH2Cl2

CH2Cl2

반응 조건

후처리

1. 1
   세척The reaction mixture was washed with H2O
2. 2
   기타dried
3. 3
   기타purified by flash column chromatography (on silica gel, CH3OH—CH2Cl2)

실험 절차

A CH2Cl2 solution (300 mL) of 3-aminopropanol (10 g, 0.133 mole) and TEA (20 g, 0.2 mole) was cooled to 0° C., followed by slow addition of CH2Cl2 solution (25 mL) of benzyl chloroformate (25 g, 0.147 mole). The resulting solution was gradually warmed to room temperature. The stirring was continued at room temperature overnight. The reaction mixture was washed with H2O, dried and purified by flash column chromatography (on silica gel, CH3OH—CH2Cl2) to yield 16.4 g, 58.9% of title compound. 1H NMR (CDCl3): δ 7.26-7.40 (m, 5H), 5.10 & 5.0-5.10 (s+m, 3H), 3.68 (q, 2H), 3.36 (q, 2H), 2.58 (t, 1H), 1.70 (p, 2H).

출처