化工社化工社 化学情報印刷レポート · 研究参考用
Water → 4-[4-(Methacryloyloxy)butoxy]benzenecarboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methacrylic Acid | HCID 4093 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 4-(4-Hydroxybutoxy)benzoic acid | HCID 15218596 | — |
| 触媒 | 2,6 Di-tert-butyl-4-(dimethylaminomethylene)phenol | HCID 86758367 | — |
| 溶媒 | 1,1,1-Trichloroethane | HCID 6278 | — |
| 生成物 | 4-[4-(Methacryloyloxy)butoxy]benzenecarboxylic acid | HCID 3720135 | 60% |
反応手順
A solution of 282 g of 4-(4′-hydroxybutoxy)benzoic acid (1.34 mol), 325 ml of freshly distilled methacrylic acid (3.35 mol), 0.3 g of 2,6 di-tert-butyl-4-(dimethylaminomethylene)phenol (Ethanox® 703) and 23.7 g of p-toluenesulfonic acid in 1.1 l of 1,1,1-trichloroethane was refluxed for 10 hours on a water separator. The reaction mixture was cooled to 60° C.-70° C. and stirred into 2.51 of petroleum ether, and the precipitate was filtered off. After washing with petroleum ether, the precipitate was dried under reduced pressure at room temperature for 24 hours, giving 223.7 g of 4-(4′-methacryloxybutoxy)benzoic acid (yield 60%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06486338B1 |
| 出典データセット | uspto-grants-2002_11 |
| ORD ID | ord-19ed3d7c5f8940d19128299bfcfcf4cd |
| 出典メモ | uspto-grants-2002_11 |