1,3-Benzothiazole-6-carboxamide → Benzothiazole-6-carbonitrile
反応式
[S:1]1[C:5]2[CH:6]=[C:7]([C:10]([NH2:12])=O)[CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1>O=P(Cl)(Cl)Cl>[S:1]1[C:5]2[CH:6]=[C:7]([C:10]#[N:12])[CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1参加物
3
実験手順
A solution of 1,3-benzothiazole-6-carboxamide (1.96 g) in POCl3 (10 ml) was refluxed for 4 hours. The reaction solution was concentrated, and water was slowly added thereto at 0° C. It was extracted with EtOAc, and the organic layer was dried over anhydrous MgSO4, and then filtered, and the filtrate was concentrated. The residue was purified by silica gel column chromatography (n-hexane:EtOAc=80:20 to 60:40) to obtain 1,3-benzothiazole-6-carbonitrile as a pale yellow solid.
後処理
- concentrationThe reaction solution was concentrated
- additionwater was slowly added
- customat 0° C
- extractionIt was extracted with EtOAc
- dry with materialthe organic layer was dried over anhydrous MgSO4
- filtrationfiltered
- concentrationthe filtrate was concentrated
- customThe residue was purified by silica gel column chromatography (n-hexane:EtOAc=80:20 to 60:40)
出典と根拠
- ORDレコード
- ord-241cd22099eb4a6b867cd58491a17d1e
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07951825B2
反応ノート
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