関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methyl-2-butanol | HCID 6405 | — |
| 反応物 | 3-Amino-1-propanol | HCID 9086 | — |
| 反応物 | 2-Chloropyridine oxide | HCID 75465 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178526251 | HCID 178526251 | 80.3% |
反応手順
A mixture of 2-chloropyridine-N-oxide (16.6 g, 100 mmoles), 3-amino-1-propanol (15.3 ml, 200 mmoles), NaHCO3 (42 g, 0.5 mole), and tert-amyl alcohol (100 ml) was heated to reflux. After 23 hours, the reaction was cooled, diluted with CH2Cl2 (300 ml), and filtered to remove insoluble materials. The filtrate was concentrated to afford a brown oil. The oil was dried under vacuum overnight. Ether (100 ml) was added to give a brown solid. The ether was decanted and the solid was washed further with ether/acetonitrile (3/1). The resulting solid was heated at 67° C. under vacuum to give the desired product (13.5 g). 1H NMR was consistent with the proposed structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06949578B2 |
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| 出典データセット | uspto-grants-2005_09 |
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| ORD ID | ord-7638cfb683b8452eb81dd8e69519514f |
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| 出典メモ | uspto-grants-2005_09 |
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