関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 6-(Trifluoromethoxy)-4-(trimethylsilyl)-2-benzothiazolamine | HCID 9972441 | — |
| 反応物 | Nitronium tetrafluoroborate | HCID 11073463 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 6-Trifluoromethoxy-4-nitro-2-benzothiazolamine | HCID 11778346 | 43.3% |
反応手順
0.68 g of nitronium tetrafluoroborate are added in small portions to a solution of 0.76 g of 2-amino-4-trimethylsilyl-6-trifluoromethoxybenzothiazole in 20 cm3 of acetonitrile cooled to 0° C. Stirring is continued for 12 hours at a temperature close to 20° C. The solution is then diluted with 50 cm3 of water and extracted with 2 times 50 cm3 of ethyl acetate. The organic phases are combined, dried over sodium sulphate and concentrated in vacuum. The residue is purified by flash chromatography on silica gel with a cyclohexane-ethyl acetate mixture (7-3 by volume) as eluent. After recrystallization from a cyclohexane-ethyl acetate mixture (3-2 by volume), 0.3 g of 2-amino-4-nitro-6-trifluoromethoxybenzothiazole melting at 260° C. is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05424439 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-3b531de0c67245a583860bb8674cac48 |
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| 出典メモ | uspto-grants-1995_06 |
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