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5-Amino-3-methylisoxazole → N-(3-methyl-5-isoxazolyl)-5-bromothiophene-2-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-Amino-3-methylisoxazole | HCID 84590 | — |
| 反応物 | 5-Bromothiophene-2-sulfonyl chloride | HCID 2733924 | — |
| 生成物 | N-(3-methyl-5-isoxazolyl)-5-bromothiophene-2-sulfonamide | HCID 22998516 | — |
反応手順
N-(3-methyl-5-isoxazolyl)-5-bromothiophene-2-sulfonamide was prepared in the same manner as described in Example 14 from 5-bromothiophene-2-sulfonyl chloride and 5-amino-3-methyl isoxazole. Purification was achieved by extraction of the crude sulfonamide into aqueous 2N NaOH, washing of the aqueous layer with ethyl acetate and acidification, using concentrated HCl, to pH ~2. Re-extraction into ethyl acetate was followed by washing of the organic material with water, brine and drying over magnesium sulfate. After evaporation of solvents, a brownish solid remained which was sufficiently pure to use in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05594021 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-f241abfbf55942dcb756a89925fcb51b |
| 出典メモ | uspto-grants-1997_01 |