関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4-Bromothiophene-2-carbaldehyde | HCID 87792 | — |
| 反応物 | Ethylorthoformate | HCID 53630039 | — |
| 生成物 | 4-Bromo-2-(diethoxymethyl)thiophene | HCID 12280024 | 81% |
反応手順
A mixture of 4-bromothiophene-2-carbaldehyde (1.2 g, 0.0063 mol) in ethanol (10 mL, 0.2 mol) was treated with ammonium chloride (0.42 g, 0.0078 mol) and ethyl orthoformate (1.2 g, 0.0078 mol). The mixture was stirred at 60° C. for 2 hours. The reaction was quenched with water and extracted with ethyl acetate. The combined organic layer was washed with saturated sodium chloride, dried over magnesium sulfate, filtered and concentrated to give 4-bromo-2-(diethoxymethyl)thiophene as an oil (1.3 g, 81%). 1H NMR (400 MHz, CDCl3): 7.22 (s, 1H), 6.99 (s, 1H), 5.68 (s, 1H), 3.63 (q, 4H) 1.24 (t, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541425B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-0cc651ffbc07409e81c77f88ad3499c1 |
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| 出典メモ | uspto-grants-2013_09 |
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