反応式
[CH3:1]C(OC(=O)C1C=CC=CC=1OCCN)C.[NH:17]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH2:19][C@H:18]1[C:26]([OH:28])=[O:27].[F:29][C:30]1[CH:35]=[CH:34][C:33]([C:36]2[CH:41]=[CH:40][C:39]([S:42](Cl)(=[O:44])=[O:43])=[CH:38][CH:37]=2)=[CH:32][CH:31]=1.CN1CCOCC1>C(#N)C>[CH3:1][O:27][C:26]([C@@H:18]1[CH2:19][C:20]2[C:25](=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:17]1[S:42]([C:39]1[CH:40]=[CH:41][C:36]([C:33]2[CH:34]=[CH:35][C:30]([F:29])=[CH:31][CH:32]=2)=[CH:37][CH:38]=1)(=[O:44])=[O:43])=[O:28]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
A mixture of 0.545 g (2.55 mmol) of the hydrochloride of the methyl ester of 2,3-dihydro-(2S)-1H-indole-2-carboxylic acid and 10 ml of acetonitrile is prepared and 0.9 g (3.32 mmol) of 4′-fluoro[1,1′-biphenyl]-4-sulfonyl chloride and 0.62 ml of N-methylmorpholine are added. The reaction mixture is stirred for 16 hours at room temperature and then concentrated under reduced pressure. The residue is taken up in 100 ml of ethyl acetate and washed with 3 times 75 ml of water. The organic phase is dried over magnesium sulfate and then concentrated under reduced pressure. The crude product is purified by chromatography on silica gel using a toluene/ethyl acetate mixture (98/2; v/v) as the eluent to give 0.83 g of the expected compound in the form of a white solid (yield=79%).
後処理
- customis prepared
- concentrationconcentrated under reduced pressure
- washwashed with 3 times 75 ml of water
- dry with materialThe organic phase is dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe crude product is purified by chromatography on silica gel using a toluene/ethyl acetate mixture (98/2; v/v) as the eluent
出典と根拠
- ORDレコード
- ord-f2a6d25bf8bd4d76b475a127cb41f42c
- 出典データセット
- uspto-grants-2008_12
- 特許番号
- US07465811B2
関連ノート
読み込み中…