関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 2,4-Pentanediol | HCID 12262 | — |
| 反応物 | Benzene, (3-chloro-1-propenyl)- | HCID 94242 | — |
| 生成物 | 2,4-Pentanediol monobenzoate monocinnamate | HCID 85856529 | 89% |
反応手順
To 0.03 mol 2,4-pentanediol were added 30 ml tetrahydrofuran and 0.04 mol pyridine, then added 0.03 mol benzoyl chloride with stirring. The reaction was heated refluxing for 4 hours, cooled. Then to the reaction were added 20 ml tetrahydrofuran and 0.05 mol pyridine, followed by 0.04 mol cinnamyl chloride with stirring. The reaction was heated refluxing for 4 hours, cooled and added 20 ml saturated saline. The reaction mixture was extracted with ethyl acetate, and the extract was dried over anhydrous sodium sulfate, filtered. After removing solvent, the crude was purified by column chromatography to give 2,4-pentanediol monobenzoate monocinnamate as a colorless liquid. The yield was 89%. 1HNMR: δ (ppm) 0.8-1.4(8H, m, CH3), 1.9-2.1(1H, m, CH), 5.1-5.3(2H, m, CH linked to ester radical), 6.2-8.0(12H, m, ArH and ═CH—)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07388061B2 |
|---|
| 出典データセット | uspto-grants-2008_06 |
|---|
| ORD ID | ord-cb7a91e2125e4369bbec1f28d17a9e49 |
|---|
| 出典メモ | uspto-grants-2008_06 |
|---|