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Isophorone diamine → 1-(1-Isobutoxycarbonyl-2-prop-1-enylamino)-3-(1-isobutoxycarbonyl-2-prop-1-enylaminomethyl)-3,5,5-trimethylcyclohexane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isophorone diamine | HCID 17857 | — |
| 反応物 | Isobutyl acetoacetate | HCID 522677 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-(1-Isobutoxycarbonyl-2-prop-1-enylamino)-3-(1-isobutoxycarbonyl-2-prop-1-enylaminomethyl)-3,5,5-trimethylcyclohexane | HCID 69858192 | 100% |
反応手順
To isophoronediamine (139.23 g, 0.819 mol) in methanol (700 ml) was slowly added with stirring isobutyl acetoacetate (262.31 g, 1.660 mol) in methanol (700 ml) over 45 minutes, during which the temperature increased from 22° C. to 30° C. The reaction mixture was allowed to stand at 21° C. overnight (15 h). Further methanol was added, and removal of solvent and drying (91° C./100 Pa) gave 1-(1-isobutoxycarbonyl-2-prop-1-enylamino)-3-(1-isobutoxycarbonyl-2-prop-1-enylaminomethyl)-3,5,5-trimethylcyclohexane (IIMTCH) as a clear light yellow viscous syrup (366.80 g, 100%), which set to a soft gum on standing and was identified by 1H-NMR, 13C-NMR, FT-IR and Raman spectra.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06521716B1 |
| 出典データセット | uspto-grants-2003_02 |
| ORD ID | ord-01d6ba5754764b41bbc2f4b9915834c2 |
| 出典メモ | uspto-grants-2003_02 |