Ethyl formate → Sodium1-ethoxy-1,3-dioxopropan-2-ide
反応式
[H-].[Na+:2].[C:3]([O:6][CH2:7][CH3:8])(=[O:5])[CH3:4].[CH:9](OCC)=[O:10]>C(OC(C)C)(C)C>[CH2:7]([O:6][C:3]([CH:4]=[CH:9][O-:10])=[O:5])[CH3:8].[Na+:2]参加物
5
反応条件
- 温度
- 45 °C
実験手順
To a suspension of sodium hydride (60% dispersion in oil) (269 g, 16.7 mol) in isopropyl ether (12 L) was slowly added ethyl acetate (1280 g, 14.2 mol) at such a rate as to maintain an internal temperature of 45° C. Ethyl formate (2232 g, 30.13 mol) then added dropwise at 42° C. and stirred at ambient temperature for 18 h. The mixture was filtered and washed with ethyl ether (2×300 mL), with hexanes (500 mL) and the solid was dried to give sodium 2-ethoxycarbonyl ethenolate as a white solid (1930 g, 99%); 1H NMR (DMSO-d6, 300 MHz) δ1.03 (t.3H), 3.86 (q, 2H), 4.08(d, 1H), 8.03 (d, 1H).
後処理
- filtrationThe mixture was filtered
- washwashed with ethyl ether (2×300 mL), with hexanes (500 mL)
- customthe solid was dried
出典と根拠
- ORDレコード
- ord-691fcef8a3be43a680687c07967da2d6
- 出典データセット
- uspto-grants-2001_09
- 特許番号
- US06294538B1
反応ノート
読み込み中…