関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methylbenzoxazole | HCID 7225 | — |
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 生成物 | 2-Methyl-1,3-benzoxazole-6-sulfonyl chloride | HCID 54593942 | 59.9% |
反応手順
Chlorosulfonic acid (12.5 ml, 187.8 mmol) was cooled in an ice bath and 2-methylbenzoxazole (5.0 g, 37.5 mmol) was carefully added drop wise over a period of 15 min. The combined mixture was heated at 115-120° C. for 16 hours. After cooling, the mixture was added very slowly to ca. 100 ml ice/water mix. The white solid that separated was collected by filtration, washed with water until washings were neutral and dried to yield 5.2 g (59%) of Compound 8, whose structure is given below:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08759526B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-19cba7e21bd745dd95faab713c599489 |
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| 出典メモ | uspto-grants-2014_06 |
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