関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methacrylic Acid | HCID 4093 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 2,3-Dihydrofuran | HCID 70934 | — |
| 触媒 | Methanesulfonic Acid | HCID 6395 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Oxolan-2-yl 2-methylprop-2-enoate | HCID 154299 | 58% |
反応手順
To a 500-mL, 3-necked round bottomed flask equipped with a thermocouple temperature monitor, nitrogen inlet and a magnetic stirrer was added 300 mL of dichloromethane, 24.5 g (0.29 mol) of methacrylic acid and 21.4 g (0.305 mol) of 2,3-dihydrofuran. The flask was cooled under Nitrogen to −40° C. and 0.05 g of methanesulfonic acid was added. The mixture was warmed to 0° C. and stirred for 6 hours at which time it was recooled to −40° C. and an excess (1 mL) of triethylamine was added. The solution was then washed with saturated sodium bicarbonate, water and brine and dried over anhydrous magnesium sulfate. Distillation from sodium carbonate at reduced pressure resulted in 26 g (58%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07820369B2 |
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| 出典データセット | uspto-grants-2010_10 |
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| ORD ID | ord-18390c950bb546b58ade338d5e6b38d8 |
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| 出典メモ | uspto-grants-2010_10 |
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