関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 1,1'-Azobis(cyclohexanecarbonitrile) | HCID 74978 | — |
| 反応物 | 5-Amino-6-fluoro-3-methyl-1,2-benzisothiazole | HCID 12056832 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 5-Amino-4-bromo-6-fluoro-3-methyl-1,2-benzisothiazole | HCID 18314499 | 101.3% |
反応手順
To a solution of 5-amino-6-fluoro-3-methyl-1,2-benzisothiazole (0.600 g, 0.00329 mol) in 1,2-dichloroethane is added N-bromosuccinimide (0.586 g, 0.00329 mol) followed by 1,1'-azobis(cyclohexanecarbonitrile) (0.0200 9). The mixture is stirred two hours at 70° C., additional N-bromosuccinimide (0.240 g, 0.00135 mol) is added, and the mixture is stirred 40 minutes at 70° C. The mixture is then cooled to room temperature, filtered and concentrated in vacua to obtain a residue. The residue is chromatographed on silica gel to give the title compound (0.870 g, 100%) which is identified by NMR spectral analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06140270 |
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| 出典データセット | uspto-grants-2000_10 |
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| ORD ID | ord-7b00408ff0314e5883ff2093a17dd602 |
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| 出典メモ | uspto-grants-2000_10 |
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