関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2(3H)-Benzoxazolone | HCID 6043 | — |
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 生成物 | 6-Benzoxazolesulfonyl chloride, 2,3-dihydro-2-oxo- | HCID 119698 | 73% |
反応手順
Benzoxazolinone (13.5 g, 0.1 mol) was added slowly to a 0° C. solution of chlorosulfonic acid (33.29 mL, 5 equivalents). The reaction was warmed to 25° C. and stirred for 0.5 h, heated to 60° C. for 3 h. The reaction was cooled to 25° C., poured into ice, filtered, and rinsed with water. The resulting white solid was redissolved in 500 mL of diethyl ether and washed with water (2×), dried over Na2SO4, filtered and concentrated to 100 mL volume. Hexane was added (100 mL) and the white precipitate was filtered and placed under vacuum to yield 17 g (73%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08193227B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-775a63dec4ee49ffa6985ad65b0364b3 |
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| 出典メモ | uspto-grants-2012_06 |
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