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Sodium Iodide → N-methyl-N-(5-nitrobenzoxazol-2-ylmethyl)-4-nitrophenethylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-(Chloromethyl)-5-nitro-1,3-benzoxazole | HCID 2764189 | — |
| 反応物 | N-methyl-4-nitrophenethylamine | HCID 2794239 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-methyl-N-(5-nitrobenzoxazol-2-ylmethyl)-4-nitrophenethylamine | HCID 19813428 | — |
反応手順
2-Chloromethyl-5-nitrobenzoxazole (2.85 g, 13.4 mmole), N-methyl-4-nitrophenethylamine (J.O.C., [1956], 21, 45) (2.2 g, 12.2 mmole), potassium carbonate (1.85 g, 13.4 mmole) and sodium iodide (2.0 g, 13.4 mmole) were heated under reflux in acetonitrile (50 ml) for 3 days. The solvent was then evaporated, the residue diluted with water, and extracted three times with methylene chloride. The combined organic extracts were washed with water, dried (MgSO4), filtered and evaporated to dryness. The resultant oil was diluted with ether and the supernatant decanted and evaporated to dryness to give an orange solid, which was recrystallised from isopropanol to give the title compound, yield 0.80 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04956382 |
| 出典データセット | uspto-grants-1990_09 |
| ORD ID | ord-4e6e03fe3c7b4e1caf2ce3299229ce73 |
| 出典メモ | uspto-grants-1990_09 |