関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Butene, 1-bromo-3-methyl- | HCID 70092 | — |
| 反応物 | 4,5-Dihydro-2,4,4-trimethyloxazole | HCID 74496 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Methoxy-3-(3-methyl-2-butenyl)-2,4,4-trimethyloxazolidine | HCID 20474260 | 86% |
反応手順
226 g (2 mols) of 2,4,4-trimethyloxazoline were dropped at room temperature to 298 g (2 mols) 3-methyl-2-butenyl bromide in 400 ml absolute methylenchloride and were stirred for 12 hours at 20° C. After cooling to 0° C. 400 ml (2 mols) of a 30% solution of sodium methylate were added and the mixture was stirred for a further hour at room temperature. The solution was filtered and after removing off the solvent the residue was distilled. 368 g (1.72 mols, 86%) of 2-methoxy-3-(3-methyl-2-butenyl)-2,4,4-trimethyloxazolidine of boiling point 70°-76° C./0.05 mm Hg were obtained. NMR (CDCL3): α1.1 (s, 3H); 1.2 (s, 3H); 1.4 (s, 3H); 1.6-1.7 (bs, 6H); 3.2 (s, 3H); 3.25 (d, J=6.5 Hz, 2H); 3.65 (s, 2H); 5.25 (t, J=6.5 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04283544 |
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| 出典データセット | uspto-grants-1981_08 |
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| ORD ID | ord-6cd0ad6f5b514f64a5ccdac555488191 |
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| 出典メモ | uspto-grants-1981_08 |
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