반응 #2833

반응 방정식

compound ( [13]-(132)-158 )

3-nitrobenzoic acid morpholide

→

compound ( [13]-(133)-158 )

수율 100.5%

3-aminobenzoic acid morpholide

수율 100.5%

용매

ethanol

hydrazine monohydrate

ethanol

반응 조건

후처리

1. 1
   기타the catalyst was removed by filtration through celite
2. 2
   농축The solution was concentrated
3. 3
   기타the residue was purified by silica gel column chromatography (Kieselgel 60=120 g, ethyl acetate)

실험 절차

The compound ([13]-(132)-158) (8.63 g) prepared in Example 83 was dissolved in ethanol (400 ml), and the solution was heated to 50° C. To the suspention, a solution of 10% Pd/C (2.25 g) in ethanol and hydrazine monohydrate (4.4 ml) were added to the solution. The mixture was stirred for 30 minutes. After the reaction was completed, the catalyst was removed by filtration through celite. The solution was concentrated, and the residue was purified by silica gel column chromatography (Kieselgel 60=120 g, ethyl acetate) to obtain the above-captioned compound ([13]-(133)-158) (7.57 g) as a white solid.

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