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Methacrylic Acid → 3'-(2-Methylacryloyloxy)biphenyl-3-yl 2-methylacrylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methacrylic Acid | HCID 4093 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | Oxalic acid dihydrate | HCID 61373 | — |
| 反応物 | 3,3'-Biphenyldiol | HCID 69165 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3'-(2-Methylacryloyloxy)biphenyl-3-yl 2-methylacrylate | HCID 58239628 | — |
反応手順
5.00 g (26.9 mmol) of biphenyl-3,3′-diol, 9.5 ml (0.112 mol) of methacrylic acid and 0.7 g of N,N-dimethylaminopyridine (DMAP) are initially introduced in 200 ml of toluene, a solution of 23.5 g (0.114 mol) of N,N′-dicyclohexylcarbodiimide is added with ice-cooling, and the mixture is stirred overnight at room temp. After addition of 4.4 g of oxalic acid dihydrate, the batch is stirred for 1 h and filtered, and the filtrate is evaporated. The residue is chromatographed on silica gel with heptane/ethyl acetate (2:1), giving 3′-(2-methylacryloyloxy)biphenyl-3-yl 2-methylacrylate as colourless crystals of m.p. 70° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08313669B2 |
| 出典データセット | uspto-grants-2012_11 |
| ORD ID | ord-c416173b03af4cec87f3da9ef56b3111 |
| 出典メモ | uspto-grants-2012_11 |