反応式
[CH3:1][N:2]([C:8]1[CH:17]=[CH:16][C:15]2[C:10](=[C:11]([CH2:18][CH2:19][NH:20][C:21](=[O:29])[CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:12]=[CH:13][CH:14]=2)[CH:9]=1)[CH2:3][CH2:4][C:5](Cl)=[O:6].[Cl-].[Al+3].[Cl-].[Cl-].Cl>ClC(Cl)C(Cl)Cl>[CH3:1][N:2]1[C:8]2[CH:17]=[CH:16][C:15]3[CH:14]=[CH:13][CH:12]=[C:11]([CH2:18][CH2:19][NH:20][C:21](=[O:29])[CH2:22][C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)[C:10]=3[C:9]=2[C:5](=[O:6])[CH2:4][CH2:3]1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 60 °C
実験手順
The product obtained in Step C (3 mmol), dissolved in 1,1,2,2-tetrachloroethane (30 ml), is added dropwise to a solution of aluminium chloride (10 mmol) in the same solvent (20 ml) under nitrogen. The reaction mixture is heated at 60° C., with stirring, until the reaction has ceased and it is then poured into a mixture of ice (10 g) and concentrated HCl (0.3 ml); stirring is continued for one hour. The aqueous phase is extracted twice with chloroform; the combined organic phases are then dried over magnesium sulphate and concentrated under reduced pressure. The residue is chromatographed on silica gel to yield the title product.
後処理
- stirringstirring
- extractionThe aqueous phase is extracted twice with chloroform
- dry with materialthe combined organic phases are then dried over magnesium sulphate
- concentrationconcentrated under reduced pressure
- customThe residue is chromatographed on silica gel
出典と根拠
- ORDレコード
- ord-6ee37953c6d04e8894e0091165d4e7c5
- 出典データセット
- uspto-grants-2006_10
- 特許番号
- US07126012B2
関連ノート
読み込み中…