関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Amino-4-chlorobenzenesulphonamide | HCID 77790 | — |
| 反応物 | 2-Butyl isothiocyanate | HCID 78151 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 178448906 | HCID 178448906 | 7% |
反応手順
A mixture of 2-amino-4-chlorobenzenesulfonamide (2.1 g, 10.16 mmol) and sec-butyl isothiocyanate (5.0 ml, 40.9 mmol) was heated at 150° C. for 4 h. The mixture was allowed to cool and then stirred with 25 ml of ethyl acetate for 1 h. The precipitate was isolated by filtration and recrystallised from ethanol to give 201 mg (7%) of the title compound as white crystals; m.p. 242-245° C.; 1H-NMR (DMSO-d6): δ 0.89 (t, 3H, CH2CH3), 1.15 (d, 3H, CHCH3), 1.50 (m, 2H, CH2), 3.76 (m, 1H, CH), 7.19 (br.s, 1H, NH), 7.29 (m, 2H, ArH), 7.68 (d, 1H,ArH), 10.35 (br.s, 1H, NH); MS: m/e 287/289 (M+); (C11H14Cl1O3S1) calc. C45.91 H, 4.90; N, 14.60; found C, 46.42; H, 5.08; N, 14.65.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06242443B1 |
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| 出典データセット | uspto-grants-2001_06 |
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| ORD ID | ord-25913c05549e4aaa8ef8897da94de8ea |
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| 出典メモ | uspto-grants-2001_06 |
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