反応式
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([S:10]([N:13]2[CH2:17][CH2:16][S:15][CH2:14]2)(=[O:12])=[O:11])[C:3]=1[C:4]#[N:5].I([O-])(=O)(=O)=[O:19].[Na+]>CO.O>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([S:10]([N:13]2[CH2:17][CH2:16][S:15](=[O:19])[CH2:14]2)(=[O:12])=[O:11])[C:3]=1[C:4]#[N:5]参加物
5
実験手順
54 mg of 2-Fluoro-6-(thiazolidine-3-sulfonyl)-benzonitrile in 10 ml of methanol and 1 ml of water are treated with 45 mg of sodium periodate, and the mixture is stirred for 14 hours at room temperature. The reaction mixture is poured into water, and the aqueous layer is extracted three times with ethyl acetate. The combined organic layers are dried over sodium sulfate, filtered and concentrated in vacuo. Purification by reverse phase HPLC affords 40 mg of 2-Fluoro-6-(1-oxo-1 lambda*4*-thiazolidine-3-sulfonyl)-benzonitrile.
後処理
- extractionthe aqueous layer is extracted three times with ethyl acetate
- dry with materialThe combined organic layers are dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customPurification by reverse phase HPLC
出典と根拠
- ORDレコード
- ord-fd5234d09edb41feb82f3dd1a0012650
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524896B2
関連ノート
読み込み中…