反応 #2833

反応方程式

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

3-nitrobenzoic acid morpholide

→

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

収率 100.5%

3-aminobenzoic acid morpholide

収率 100.5%

溶媒

ethanol

hydrazine monohydrate

ethanol

反応条件

後処理

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

実験手順

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.

出典