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Dichloromethane → 2-bromo-N-tert-butylbenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Tert-Butylamine | HCID 6385 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Bromobenzenesulfonyl chloride | HCID 520403 | — |
| 生成物 | 2-bromo-N-tert-butylbenzenesulfonamide | HCID 4825014 | 97.1% |
反応手順
2-Bromobenzenesulfonyl chloride (100.9 g, 394.9 mmol) was dissolved in methylene chloride (500 mL, 8.0 mol) and cooled at 0° C. t-Butylamine (41.3 mL, 395 mmol) was added in 3 portions over approximately 1 minute. DIPEA (75.7 mL, 434 mmol) was immediately added in 3 portions over approximately 1 minute. The mixture was warmed to room temperature and stirred overnight. The product was washed with 1M H3PO4 (2×), with saturated. NaHCO3, and with saturated aqueous NaCl, then dried over MgSO4, filtered, and concentrated to yield 2-bromo-N-t-butyl-benzenesulfonamide (112 g) as a light brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822522B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-a7f123144a76456fad9d82b6c413cc94 |
| 出典メモ | uspto-grants-2014_09 |