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Benzoic Acid → 3-(4-Tert.butyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoic Acid | HCID 243 | — |
| 反応物 | Ethyl 2-(triphenylphosphoranylidene)propionate | HCID 79792 | — |
| 反応物 | Cyclohexanecarboxaldehyde, 4-(1,1-dimethylethyl)- | HCID 88655 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Methanol--water (1/1) | HCID 22242641 | — |
| 生成物 | 3-(4-Tert.butyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester | HCID 56989205 | — |
反応手順
A mixture of 20.2 g of 4-tert.butyl-cyclohexane-1-carboxaldehyde, 52 g of (α-carbethoxy-ethylidene)-triphenyl-phosphorane and 3.6 g of benzoic acid in 120 ml of toluene is heated at reflux for 16 hours under nitrogen gasification and the toluene is evaported. The oily-crystalline residue is dissolved in 600 ml of methanol/water (4:1) and exhaustively extracted with hexane. The combined hexane extracts are washed with sodium bicarbonate solution and water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 3-(4-tert.butyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester of boiling point 99° C./0.03 Torr.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04241058 |
| 出典データセット | uspto-grants-1980_12 |
| ORD ID | ord-371e8a1fcf7f4418af5fe2f16400894e |
| 出典メモ | uspto-grants-1980_12 |