تفاعل #1328393

معادلة التفاعل

benzyl chloroformate

3-aminopropanol

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title compound

المردود 58.9%

N-CBZ-3-aminopropanol

المردود 58.9%

المذيبات

CH2Cl2

CH2Cl2

ظروف التفاعل

المعالجة

1. 1
   غسيلThe reaction mixture was washed with H2O
2. 2
   أخرىdried
3. 3
   أخرىpurified by flash column chromatography (on silica gel, CH3OH—CH2Cl2)

الإجراء التجريبي

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).

المصدر