関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tert-Butyl nitrite | HCID 10906 | — |
| 反応物 | Methyl 2-amino-5-phenylthiophene-3-carboxylate | HCID 705256 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 5-phenylthiophene-3-carboxylate | HCID 819151 | 100% |
反応手順
To a solution of tert-butyl nitrite (428 μL, 3.6 mmol) in N,N-dimethylformamide (5 mL) at 60° C. was dropwise added a solution of methyl 2-amino-5-phenylthiophene-3-carboxylate (11a) (420 mg, 1.8 mmol) in N,N-dimethylformamide (2.5 mL). The mixture was stirred at 60° C. for 1 hour, poured in water (15 mL) and extracted with ethyl acetate (2×20 mL). The organic layer was washed with brine (2×10 mL), dried over sodium sulfate and concentrated in vacuo. The residue was dissolved in toluene (5 mL) and concentrated in vacuo to provide the desired product (11b) (390 mg, 1.8 mmol, 99%) which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09238026B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-c9133882019c4cfa83115013489f40ff |
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| 出典メモ | uspto-grants-2016_01 |
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