تفاعل #2833

معادلة التفاعل

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

3-nitrobenzoic acid morpholide

→

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

المردود 100.5%

3-aminobenzoic acid morpholide

المردود 100.5%

المذيبات

ethanol

hydrazine monohydrate

ethanol

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر