関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dibenzylamine | HCID 7656 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Bromobenzenesulfonyl chloride | HCID 520403 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N,N-dibenzyl-2-bromobenzenesulfonamide | HCID 3731394 | 88.5% |
反応手順
2-Bromobenzenesulfonyl chloride (1.0 g, 3.91 mmol) and triethylamine (455 mg, 0.63 mL, 4.5 mmol) were dissolved in THF (15 mL), and the mixture was cooled to 10° C. Dibenzylamine (849 mg, 0.83 mL, 4.3 mmol) was then added dropwise. The cooling bath was removed, and the reaction mixture was stirred for 10 h at rt and then an additional 6 h at 60° C. After cooling to rt, the solvent was removed under reduced pressure, and ethyl acetate was added. The organic layer was successively washed with 1N HCl, water, semi-saturated aq Na2CO3 solution, water, and brine. After drying with Na2SO4 and filtration, the solvent was removed under reduced pressure to afford the title compound as off-white crystals (1.44 g, 88%). 1H NMR (400 MHz, CDCl3) δ 4.42 (s, 4H), 7.08 (m, 4H), 7.27 (m, 6H), 7.41 (m, 2H), 7.78 (d, 1H), 8.19 (d, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07265144B2 |
|---|
| 出典データセット | uspto-grants-2007_09 |
|---|
| ORD ID | ord-f9d57061d5ba4f5dae8ec74d4cd78720 |
|---|
| 出典メモ | uspto-grants-2007_09 |
|---|