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Methyl 5-((hydroxyimino)methyl)thiophene-2-carboxylate → HCID 14871948、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 5-((hydroxyimino)methyl)thiophene-2-carboxylate | HCID 72740488 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | HCID 14871948 | HCID 14871948 | 99.7% |
反応手順
A solution of methyl 5-((hydroxyimino)methyl)thiophene-2-carboxylate (440 mg, 2.4 mmol) in acetic anhydride (10 mL) was refluxed for 16 h. After completion, the reaction mixture was cooled to room temperature, concentrated under reduced pressure and the residue was dissolved in diethyl ether. The organic layer was washed with 10% aqueous NaOH solution, water and brine, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure to yield methyl 5-cyanothiophene-2-carboxylate (5-cyano-thiophene-2-carboxylic acid methyl ester) (400 mg, yield 90%) which was carried through without any further purification. 1H NMR (400 MHz, DMSO-d6) δ 7.77 (d, J=4.2 Hz, 1H), 7.60 (d, J=4.1 Hz, 1H), 3.95 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08901156B2 |
| 出典データセット | uspto-grants-2014_12 |
| ORD ID | ord-a5fb5d6652714366a689781b8c78d6d9 |
| 出典メモ | uspto-grants-2014_12 |