関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylorthoformate | HCID 53630039 | — |
| 反応物 | 4,5-Dichloro-2-cyclopropylaminobenzenesulphonamide | HCID 67529833 | — |
| 生成物 | 6,7-dichloro-4-cyclopropyl-4H-1,2,4-benzothiadiazine 1,1-dioxide | HCID 67530650 | — |
反応手順
In a round-bottom flask, a mixture of 4,5-dichloro-2-cyclopropylaminobenzenesulphonamide from the Step above (2.5 g) and ethyl orthoformate (25 mL) is heated in the open state at 150° C. for 1 hour. The suspension obtained is cooled on an ice bath, and the insoluble material is collected by filtration, washed with ether and dried. The solid is re-dissolved in a mixture of acetone and methanol in the hot state and the hot solution is treated with absorbent carbon and then filtered and concentrated to dryness. The residue is recrystallised from methanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741320B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-7b7f45fc90a3465183bb7ac4ccf35df4 |
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| 出典メモ | uspto-grants-2010_06 |
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