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2,6-Pyridinedimethanol → 2,6-Diformylpyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Pyridinedimethanol | HCID 70957 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2,6-Diformylpyridine | HCID 79485 | 858.1% |
反応手順
This preparation procedure followed the literature procedure (J. Chem. Soc., Dalton Trans. 1984-1937). To the mixture of 11.51 g of 2,6-pyridine-dimethanol (8.28 mmol) and 9.99 g of SeO2, was added 200 mL of 1,4-dioxane. The mixture was then refluxed for 4 h and filtered. The filtrate was concentrated under reduced pressure. The solid was dissolved in CH2Cl2 and passed through a silica gel plug. The solution was concentrated, and the solid was recrystallized from 60 mL of acetone and 100 mL of hexanes to afford 9.6 g of white crystal (71%), which was kept under N2. 1H NMR (CDCl3) δ 8.02-8.12 (m, 3H), 10.08 (s, 2H), 13C NMR δ 125.7, 138.8, 153.3, 192.7.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06380392B1 |
| 出典データセット | uspto-grants-2002_04 |
| ORD ID | ord-0360aa58883b4023a40e4b88e037091d |
| 出典メモ | uspto-grants-2002_04 |