関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Chloro-2-butanone | HCID 80608 | — |
| 反応物 | Benzosulfinide sodium; Garantose sodium | HCID 24181110 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(3-Oxobutyl)-1H-1lambda~6~,2-benzothiazole-1,1,3(2H)-trione | HCID 13059140 | 86.1% |
反応手順
9.0 g (76 millimoles) of 4-chlorobutan-2-one were slowly added dropwise to 10.0 g (50 millimoles) of sodium saccharin in 100 ml of absolute dimethylformamide, while stirring. The temperature was then gradually increased to 80° C., and the reaction mixture was stirred at this temperature for 5 hours, after which it was cooled. An excess of ice-water was added, and stirring was continued for a further hour. The precipitated solid was filtered off under suction, recrystallized from ethanol and dried in a drying oven under reduced pressure at 50° C. to give 10.9 g (86%) of N-(2-oxobut-4-yl)-saccharin of melting point 118°-119° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04563474 |
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| 出典データセット | uspto-grants-1986_01 |
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| ORD ID | ord-e7f692a0142d437890f7a7c8ff945789 |
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| 出典メモ | uspto-grants-1986_01 |
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