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Nitric Acid → 2,6-Lutidine, 4-nitro-, 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | 2,6-Dimethylpyridine N-oxide | HCID 14083 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 2,6-Lutidine, 4-nitro-, 1-oxide | HCID 20945 | 76% |
反応手順
A solution of 2.23 g (18.1 mmol) of 2,6-dimethylpyridine 1-oxide (Alfa Aesar) in 7 mL of H2SO4 and 2.7 mL of HNO3 was stirred at 130° C. for 23.5 h. The solution was added to ice with CHCl3 and H2O, and the aqueous layer was extracted with CHCl3 (2×). The combined extracts were washed with 75 mL of saturated NaHCO3 solution, and the aqueous layer was extracted with CHCl3. The combined extracts were washed with brine, dried over Na2SO4, filtered, and concentrated to give 2.3 g of 2,6-dimethyl-4-nitropyridine 1-oxide in 76% yield which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08299267B2 |
| 出典データセット | uspto-grants-2012_10 |
| ORD ID | ord-7294282d81874981a4d8835a09f100bd |
| 出典メモ | uspto-grants-2012_10 |