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Triethylamine → 2-Dimethylaminopyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methacrylic anhydride | HCID 12974 | — |
| 反応物 | 2-Methyl-2-adamantanol | HCID 136545 | — |
| 反応物 | Tempo | HCID 2724126 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Dimethylaminopyridine | HCID 21885 | 40% |
反応手順
A glass flask equipped with a stirrer, two dropping funnels, a thermometer and a Dimroth condenser was charged with 16.6 g (0.1 mol) of 2-methyl-2-adamantanol, 23.1 g (0.15 mol) of methacrylic anhydride of 97% purity which is obtained by the process of example 1, 15.7 g (0.155 mol) of triethylamine, 0.6 g (0.005 mol) of dimethylaminopyridine, 70 ml of toluene and 0.005 g of HO-TEMPO, and the mixture was heated and stirred at 50° C. for 31 hours. It was confirmed that 2-methyl-2-adamantyl methacrylate was formed in the reaction mixture in a yield of about 40%. The resultant 2-methyl-2-adamantyl methacrylate was chromatographed on silica gel to obtain 9.1 g of 2-methyl-2-adamantyl methacrylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06642394B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-659aad3e821c46a8bb7a614ad8a38e1e |
| 出典メモ | uspto-grants-2003_11 |