反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]2[CH2:14][NH:13][CH2:12][CH2:11][NH:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].[CH3:15][C:16]1[CH:17]=[C:18]([CH:22]=[C:23]([CH3:25])[CH:24]=1)[C:19](O)=[O:20].O.ON1C2C=CC=CC=2N=N1.CCN(CC)CC>C(Cl)Cl>[CH3:15][C:16]1[CH:17]=[C:18]([CH:22]=[C:23]([CH3:25])[CH:24]=1)[C:19]([N:13]1[CH2:12][CH2:11][NH:10][CH:9]([C:4]2[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=2)[CH2:14]1)=[O:20]参加物
実験手順
To a cooled solution of CH2Cl2 (600 mL) containing 2-(3,4-dichlorophenyl)piperazine (6.934 g, 30 mmol), 3,5-dimethylbenzoic acid (4.55 g, 30 mmol), and N-hydroxybenzotriazole monohydrate (4.05 g, 30 mmol) at -20° C. were added Et3N (4.2 mL, 30 mmol) and N,N-dimethylaminopropylethylcarbodimide (DEC) (5.86 g, 30 mmol) under nitrogen. The reaction was kept at -20° C. for an hour and gradually warmed to RT overnight. After stirring 22 hours, the reaction was complete and CH2Cl2 (200 mL) was added. The organic solution was washed with brine (150 mL, 3×), dried over MgSO4, filtered and concentrated under vacuum to give 8.2 g of crude product. The product was crystallized from CH2Cl2 /Hexane to give a light yellow solid (6.3 g, 17.34 mmol, 57.8%). Mm.p.139-141° C.; FAB MS [M+1]+35Cl 363.1.
後処理
- waitThe reaction was kept at -20° C. for an hour
- washThe organic solution was washed with brine (150 mL, 3×)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated under vacuum
- customto give 8.2 g of crude product
- customThe product was crystallized from CH2Cl2 /Hexane
出典と根拠
- ORDレコード
- ord-f83c28f0b5ee407aa13c4f0398fad8a3
- 出典データセット
- uspto-grants-2000_04
- 特許番号
- US06051575
関連ノート
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