関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | N-tert-butyl-2-methylpropan-1-amine | HCID 527145 | — |
| 生成物 | tert-Butylisobutylmethylamine | HCID 23381579 | — |
反応手順
A 37% solution of formaldehyde (6.89 g, 85 mmol) was added dropwise to a mixture of tert-butylisobutylamine (10.00 g, 77 mmol) and 88% formic acid (7.85 g, 0.15 mol) at room temperature. The mixture was heated at 50-55° C. for 5 h. Aqueous 8 M potassium hydroxide (12.5 ml, 0.1 mol) was added, the organic layer was separated and the aqueous layer was extracted with n-pentane (50 ml). The extract was combined with the organic layer and dried over anhydrous magnesium sulfate. The product was isolated by distillation to yield 9.25 g, (84%), bp 44-45° C./18 mm Hg; 1H NMR (CDCl3) δ0.85 (d, J=6.7 Hz, 6H, CH3), 1.01 (s, 9H, CH3), 1.64 (nonet, J=6.7 Hz, 1H, CH), 2.02 (d, J=6.7 Hz, 2H, CH2), 2.15 (s, 3H, CH3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06248885B1 |
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| 出典データセット | uspto-grants-2001_06 |
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| ORD ID | ord-ae6f33fa3f5645808032d654ba607712 |
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| 出典メモ | uspto-grants-2001_06 |
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