反応式
[NH:1]([C:3]1[CH:4]=[N:5][CH:6]=[CH:7][CH:8]=1)[NH2:2].[Cl:9][C:10]1[CH:11]=[C:12]([CH:24]=[CH:25][CH:26]=1)[C:13]([CH:15]([C:21](=O)[CH3:22])[CH2:16][C:17]([O:19][CH3:20])=[O:18])=O>C(O)C>[Cl:9][C:10]1[CH:11]=[C:12]([C:13]2[N:1]([C:3]3[CH:4]=[N:5][CH:6]=[CH:7][CH:8]=3)[N:2]=[C:21]([CH3:22])[C:15]=2[CH2:16][C:17]([O:19][CH3:20])=[O:18])[CH:24]=[CH:25][CH:26]=1参加物
4
反応条件
- 温度
- 130 °C
実験手順
0.577 g (4.233 mmol) of 3-hydrazinopyridine in 5.00 ml of ethanol was added to 0.650 g (2.419 mmol) of methyl 3-(3-chlorobenzoyl)-4-oxopentanoate, and the mixture was stirred in a closed vessel in a microwave oven at 130° C. for 1.5 h. The solvent was removed under reduced pressure, and the residue was taken up in dichloromethane and washed twice with in each case 25 ml of water. The combined organic phases were dried over sodium sulfate, and the solvent was removed under reduced pressure. Chromatography of the residue gave 0.364 g (42% of theory) of a light-yellow oil. 1H-NMR (CDCl3): see Table 2.
後処理
- customThe solvent was removed under reduced pressure
- washwashed twice with in each case 25 ml of water
- dry with materialThe combined organic phases were dried over sodium sulfate
- customthe solvent was removed under reduced pressure
- customChromatography of the residue gave 0.364 g (42% of theory) of a light-yellow oil
出典と根拠
- ORDレコード
- ord-76739736b14c447e83fa235c27e92d13
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08252723B2
関連ノート
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