関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Ethyl p-methylbenzenesulfonate | HCID 6638 | — |
| 反応物 | 5-Hexylsulfonamido-2-methylbenzoxazole | HCID 15051064 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Ethyl-5-hexylsulfonamido-2-methylbenzoxazolium p-toluenesulfonate | HCID 19993452 | 23% |
反応手順
A mixture of 60 grams (0.2 Mol) 5-hexylsulfonamido-2-methylbenzoxazole and 44 grams (0.22 Mol) ethyl p-toluenesulfonate was heated in a round bottom flask at 150° C. for 5 minutes. Upon cooling to room temperature the crude brown mass almost solidified. The product was dissolved in 25 mL methanol and poured into 300 mL diethyl ether with rapid stirring for one hour. The solid precipitate was chilled at 2° C. for 12 hours, then filtered. The tan powder was thoroughly washed with ether and recrystallized from 200 mL hot isopropyl alcohol to yield 23.4 grams (47 mMol, 23% yield) of white crystalline product, m.p.=159°-161° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05055387 |
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| 出典データセット | uspto-grants-1991_10 |
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| ORD ID | ord-3643c870cb7b4b4b897b06fdf136c84a |
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| 出典メモ | uspto-grants-1991_10 |
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