関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium acrylate | HCID 4429391 | — |
| 反応物 | 1-Chloroethyl 4-acryloyloxybutyl carbonate | HCID 53913051 | — |
| 触媒 | 18-Crown-6 | HCID 28557 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Acryloyloxyethyl 4-acryloyloxybutyl carbonate | HCID 53961440 | 89.4% |
反応手順
1-Chloroethyl 4-acryloyloxybutyl carbonate (1.253 g, 5.00 mmol) is added to a suspension of freeze dried potassium acrylate (0.606 g, 5.50mmol) and 18-crown-6 (0.066 g, 0.25 mmol) in dimethylformamide (50 ml) under a dry N2 atmosphere. After 5 days at 20° C. the solvent is removed under reduced pressure and the residue dissolved by adding dichloromethane (60 ml) and water (30 ml). After separating the phases the aqueous layer is extracted with dichloromethane (3×30 ml) and the combined organic phase washed with saturated aqueous sodium hydrogen carbonate (50 ml). The organic phase is dried (MgSO4) and the solvent removed under reduced pressure to give 1.28 g (89%) of the title product. 1H NMR (60 MHz, CDCl3): δ1.58 (3H, d, J=5 Hz, CH3 --CH), 1.80 (4H, m, CH2 --CH2), 4.24 (4H, m, 2×CH2 --O), 5.7-6.7 (6H, m, 2×CH=CH2), 6.87 (1H, k, J=5 Hz, CH--CH3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05693321 |
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| 出典データセット | uspto-grants-1997_12 |
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| ORD ID | ord-f060e74fb5b746cbb03a0cb4ee0b1881 |
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| 出典メモ | uspto-grants-1997_12 |
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