반응 #7012

반응 방정식

hydrazine

tert-butyl malonate

1-hydroxybenzotriazole hydrate

triethylamine

1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride

→

title compound

3-Oxo-3-[N′-(3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-4-carbonyl)-hydrazino]-propionic acid tert-butyl ester

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   세척washed with water (150 ml)
2. 2
   건조dried (MgSO4)
3. 3
   기타evaporated under reduced pressure
4. 4
   기타The residual oil was purified by column chromatography on silica gel

실험 절차

A mixture of the hydrazine from preparation 35 (2.2 g, 10 mmol), tert-butyl malonate (1.6 g, 10 mmol), 1-hydroxybenzotriazole hydrate (2.02 g, 15 mmol), triethylamine (4.8 ml, 20 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.4 g, 12.5 mmol) in dichloromethane (50 ml) was stirred at room temperature for 5 hours. The reaction was diluted with dichloromethane (200 ml), washed with water (150 ml), dried (MgSO4) and evaporated under reduced pressure. The residual oil was purified by column chromatography on silica gel using ethyl acetate as eluant to afford the title compound, as a white solid, 1.4 g.

출처