Hydrochloric Acid → Ethyl 2-benzoyl-6chloro-3-[(methoxycarbonyl)amino]-1H-indole-1-caboxylate
反応式
[NH2:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[Cl:11])[N:4]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:3]=1[C:17](=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.N1C=CC=CC=1.Cl[C:32]([O:34][CH3:35])=[O:33].Cl>ClCCl>[C:17]([C:3]1[N:4]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:5]2[C:6]([C:2]=1[NH:1][C:32]([O:34][CH3:35])=[O:33])=[CH:7][CH:8]=[C:9]([Cl:11])[CH:10]=2)(=[O:24])[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1参加物
6
実験手順
To a solution of ethyl 3-amino-2-benzoyl-6-chloro-1H-indole-1-caboxylate (step 2, 1.5 g, 4.4 mmol) and pyridine (0.50 ml, 6.6 mmol) in dichloromethane (20 ml) was added methyl chloroformate (0.40 ml, 5.3 mmol) at room temperature. After stirring for 3 h, the mixture was poured into 2N aqueous HCl (20 ml) and extracted with dichloromethane (30 ml×2). The combined organic layers were dried (MgSO4) and concentrated to give 1.7 g (quant.) of the title compound as yellow amorphous solids.
後処理
- extractionextracted with dichloromethane (30 ml×2)
- dry with materialThe combined organic layers were dried (MgSO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-e3ffb8b046704cd18cae7894ae1e9c42
- 出典データセット
- uspto-grants-2001_08
- 特許番号
- US06277878B1
反応ノート
読み込み中…