関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,4-Dichloro-1,3,5-triazine | HCID 17810 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (3-Aminophenyl)methanesulfonamide | HCID 13266255 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-[(4-Chloro-1,3,5-triazin-2-yl)amino]benzenemethanesulfonamide | HCID 86679822 | — |
反応手順
To a solution of 2,4-dichloro-1,3,5-triazine (1.0 eq) in dry DMF (0.7 M) at 0° C. under N2 atmosphere was added a solution of (3-aminophenyl)-methanesulfonamide (1.0 eq) in dry DMF (0.7 M). The reaction mixture was stirred for 2.5 h at 0° C. Then water was added and the aqueous solution was neutralized with sat. aq. NaHCO3 solution. The aqueous layer was extracted with EtOAc and the combined organic layers were dried over Na2SO4. Evaporation of solvent gave A1 as a white solid which was used in the next step without further purification. 1H NMR (400 MHz, d6-DMSO, 300K) δ 4.26 (s, 2H), 6.89 (s, 2H), 7.15 (d, J=7.4 Hz, 1H), 7.36 (d, J=7.4 Hz, 1H), 7.66 (d, J=7.4 Hz, 1H), 8.64 (s, 1H), 9.75 (br. s, 1H), 10.83 (s, 1H). MS (ES) C10H10ClN5O2S requires: 299. found: 300 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09226929B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-4c537d3662694d899423edc50d09fd9b |
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| 出典メモ | uspto-grants-2016_01 |
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