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Dimethylformamide → HCID 13051485、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 1-methoxy-N,N,N',N'-tetramethylmethylenediamine | HCID 70908 | — |
| 反応物 | Dimethylformamide diethylacetal | HCID 70913 | — |
| 反応物 | 2-(2H-1,4-benzothiazin-3(4H)-ylidene)-2-(4-fluorophenyl)acetamide | HCID 70532585 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 13051485 | HCID 13051485 | — |
反応手順
To 4 parts of 2-(2H-1,4-benzothiazin-3(4H)-ylidene)-2-(4-fluorophenyl) acetamide in 80 parts of DMF is added 6 parts dimethylformamide diethyl acetal and the reaction mixture was stirred at room temperature for 2 to 6 hours then heated at 80°-140° C. for 1 to 6 hours. After cooling 6 parts of methoxy-bis-(dimethylamino) methane is added and the reaction mixture then heated at 50° to 80° C. for 2 to 24 hrs. The cooled reaction mixture is then diluted with 40 parts of water and refluxed for 2 to 18 hr. Upon cooling the precipitate present was collected and recrystallized from aqueous DMF to give 4-(4-fluorophenyl)-5H-pyrido[3,4-b][1,4]benzothiazin-3(2H)-one which melts above 300°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04356302 |
| 出典データセット | uspto-grants-1982_10 |
| ORD ID | ord-a66c3ba75bfd48adb4984e20dbc5427e |
| 出典メモ | uspto-grants-1982_10 |