関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Hydroxyethyl Methacrylate | HCID 13360 | — |
| 反応物 | Hexahydro-4-methylphthalic anhydride | HCID 86876 | — |
| 反応物 | Methylhexahydrophthalic anhydride | HCID 3016472 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 生成物 | 4-Methyl-(2-methacryloyloxyethyl)hexahydrophthalic acid | HCID 67451049 | — |
反応手順
2-Methyl-hexahydrophthalic anhydride (Also known as 4-methyl-1,2-cyclohexanedicarboxylic anhydride; 210.0 g, 1.25 mol, CAS #19438-60-9, Alfa Aesar, lot B04w039), 4-(dimethylamino)pyridine (DMAP, 7.5 g, 0.06 mol, CAS #1122-58-3, Alfa Aesar, lot L125009), 2-hydroxyethylmethacrylate (HEMA, 162.5 g, 1.25 mol, and butylated hydroxytoluene (BHT, 0.380 g) were charged into a 1-liter 3-neck reaction flask equipped with a mechanical stirrer, a thermocouple connected to a temperature controller, a dry air stream running through a T-shape connection into the reactor then to an oil bubbler, and a heating mantle. The mixture was continuously stirred at 95° C. for 5 hours. The heat was turned off and the flask contents were allowed to cool to room temperature to give 4-methyl-(2-methacryloyloxyethyl)hexahydrophthalic acid intermediate as a colorless viscous liquid. Structure was confirmed by NMR.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09237990B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-222968c009a4419199ad1364d2fb2a69 |
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| 出典メモ | uspto-grants-2016_01 |
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