関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | 5-Acetyl-2-bromopyridine | HCID 15668195 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Bromo-5-(2-methyl-1,3-dioxolan-2-yl)pyridine | HCID 85775099 | 79% |
反応手順
A mixture of 5-acetyl-2-bromopyridine (0.6 g, 3.00 mmol), ethylene glycol (0.535 ml, 9.60 mmol), p-toluenesulfonic acid monohydrate (0.171 g, 0.900 mmol), and toluene (12.00 ml) was stirred at 140° C. for 5 hours. The reaction mixture was washed with saturated sodium bicarbonate and brine. The aqueous layer was back extracted with ethyl acetate and the combined organics dried with magnesium sulfate and concentrated to give crude 2-bromo-5-(2-methyl-1,3-dioxolan-2-yl)pyridine (0.575 g, 2.356 mmol, 79% yield) as an orange oil. It 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 | US09174992B2 |
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| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-709de68ecef14f7bb3f15a90f7ea0293 |
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| 出典メモ | uspto-grants-2015_11 |
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