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N-(4-(4-methoxybenzyloxy)-3-(3-trifluoromethylphenyl)benzyl)-4-fluoro-N-methylbenzenesulfonamide → N-(3-(3-trifluoromethylphenyl)-4-hydroxybenzyl)-4-fluoro-N-methylbenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-(4-(4-methoxybenzyloxy)-3-(3-trifluoromethylphenyl)benzyl)-4-fluoro-N-methylbenzenesulfonamide | HCID 66868532 | — |
| 溶媒 | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| 生成物 | N-(3-(3-trifluoromethylphenyl)-4-hydroxybenzyl)-4-fluoro-N-methylbenzenesulfonamide | HCID 66868277 | 64% |
反応手順
Intermediate 35 (700 mg, 1.25 mmol) was dissolved in TFA/DCM (1/1) and stirred at room temperature for 1 h. Solvent was removed in vacuo and the residue was purified via silica gel chromatography (0-40% EtOAc/hexane) to afford 350 mg (64%) of N-(3-(3-trifluoromethylphenyl)-4-hydroxybenzyl)-4-fluoro-N-methylbenzenesulfonamide (36). 1HNMR (CD3OD, 400 MHz): δ 7.91 (m, 2H), 7.80 (s, 1H), 7.65 (m, 2H), 7.59 (d, 1H), 7.15-7.25 (m, 4H), 6.94 (d, 1H), 4.97 (s, 1H), 4.13 (s, 2H), 2.64 (s, 3H). MS (ESI): MH+=440.1. HPLC (Method B) tR=3.45 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822467B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-089e0588540140d9bcdba89eff06b05e |
| 出典メモ | uspto-grants-2014_09 |