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Thiophene → 3-oxo-2-(2-thienyl)-3,4-dihydro-2H-1,4-benzothiazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiophene | HCID 8030 | — |
| 反応物 | 2H-1,4-Benzothiazin-3(4H)-one, 2-chloro- | HCID 12218599 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-oxo-2-(2-thienyl)-3,4-dihydro-2H-1,4-benzothiazine | HCID 18984406 | 70.3% |
反応手順
To a solution of 2-chloro-3-oxo-3,4-dihydro-2H-1,4-benzothiazine (9.38 g) and thiophene (7.91 g) in methylene chloride (250 ml) is added in portions stannic chloride (12. 2 g) at 0° to 5° C. After stirring at the same temperature for 45 minutes, the mixture is poured into ice water, and the organic layer is separated. The aqueous layer is extracted with ethyl acetate, and the ethyl acetate layer is combined with the above organic layer and distilled to remove the solvent. The resulting solid material is recrystallized from ethanol to give 3-oxo-2-(2-thienyl)-3,4-dihydro-2H-1,4-benzothiazine (8.17 g) as crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246929 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-9f13dedfca454f268811c8281667b82c |
| 出典メモ | uspto-grants-1993_09 |