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Chlorosulfonic acid → 5-Bromo-2-oxo-2,3-dihydro-1,3-benzoxazole-6-sulfonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | 2-Benzoxazolinone, 5-bromo- | HCID 26853 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Bromo-2-oxo-2,3-dihydro-1,3-benzoxazole-6-sulfonyl chloride | HCID 12611046 | — |
反応手順
To a mixture of commercially-available 5-bromobenzo[d]oxazol-2(3H)-one (35-1, 500 mg, 2.336 mmol) in DCM (23 mLl) at RT was added chlorosulfonic acid (1565 μl, 23.36 mmol). The mixture became a solution that was stirred at RT. After 18 h, The solution was cooled to 0° C. and carefully quenched with ice chips and then partitioned between water (15 mL) and EtOAc (150 mL). The aqueous layer was extracted with 3×30 mL DCM. The combined organics were dried over Na2SO4, filtered, concentrated to give 35-2 as a white solid, which was carried forward without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09273040B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-7a9772516b7644b49473e9d2e760556d |
| 出典メモ | uspto-grants-2016_03 |