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Pyridine → 1,2-Benzenedimethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 1,4-Benzenedimethanol | HCID 11506 | — |
| 反応物 | Isobutyryl chloride | HCID 62325 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 1,2-Benzenedimethanol | HCID 69153 | 212.9% |
反応手順
1,4-xylylene glycol (5 g, 0.0306 mol), pyridine (5.7 g, 0.072 mol), and catalyst DMAP (ca. 100 mg) in a solution of dichloromethane (ca. 25 ml) were added to a flask. Isobutyryl chloride (7.71 g, 0.072 mol) was then added to the solution drop wise. The mixture was stirred overnight. 1M HCL brine was used to wash the mixture. The organic layer was dried over MgSO4 and concentrated in vacuo to afford a clear oil as the product (9 g). Its purity was ascertained using 1H NMR (300 MHz in CDCL3): δ 7.34 (s, 4H), 5.11 (s, 4H), 2.60 (sept, 2H), 1.19 (d, 12H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09340658B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-709dbd25a92f41c0adc014e5dfe877dd |
| 出典メモ | uspto-grants-2016_05 |