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Sodium Iodide → HCID 23365874、化合物
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 | Methyl 3-(bromomethyl)benzoate | HCID 517981 | — |
| 反応物 | 6-nitro-3,4-dihydro-2H-1,4-benzoxazine | HCID 7062225 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | HCID 23365874 | HCID 23365874 | 85% |
反応手順
A mixture of 6-nitro-2,3-dihydrobenz-1,4-oxazine (0.45 g.), methyl 3-bromomethylbenzoate* (Y) (0.58 g.), potassium carbonate (0.35 g.), and sodium iodide (0.38 g.) in dry 2 -butanone (25 ml.) was stirred and heated under reflux for 48 hours. The cooled reaction mixture was filtered, the filter cake washed with 2-butanone, and the combined filtrate evaporated. The product was purified by flash chromatography on silica gel, eluting with 5:95 v/v ethyl acetate:toluene to give methyl 3-(6-nitro-2,3-dihydrobenz-1,4-oxazin-4-ylmethyl)benzoate (0.7 g., 85%) as a yellow oil; partial NMR (80 MHz, CDCl3): 3.5(m,2H, N.CH2.CH2O); 3.9(s,3H, OMe); 4.3(m,2H, N.CH2.CH2O); 4.6(s,2H, NCH2Ar).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05391758 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-01cf757aae454869b671e8ce81965cb2 |
| 出典メモ | uspto-grants-1995_02 |