反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:15]=[CH:16][CH:17]=1)[C:7]([N:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1)=[O:8])([O-])=O>C(O)C.O.NN.[Pd]>[NH2:1][C:4]1[CH:5]=[C:6]([CH:15]=[CH:16][CH:17]=1)[C:7]([N:9]1[CH2:10][CH2:11][O:12][CH2:13][CH2:14]1)=[O:8]参加物
5
反応条件
- 温度
- 50 °C
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.
後処理
- customthe catalyst was removed by filtration through celite
- concentrationThe solution was concentrated
- customthe residue was purified by silica gel column chromatography (Kieselgel 60=120 g, ethyl acetate)
出典と根拠
- ORDレコード
- ord-7cc7d41500194b2d804cca39c54e96aa
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05731310
関連ノート
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