Ethyl Acetate → Ethyl 2-methyl-1,3-oxazole-4-carboxylate
反応式
[CH2:1]([O:3][C:4]([C:6]([N:9]=[C:10]([O:12][CH2:13]C)[CH3:11])=C[O-])=[O:5])[CH3:2].[K+].CCOC(C)=O.C([O-])(O)=O.[Na+]>C(O)(=O)C>[CH2:1]([O:3][C:4]([C:6]1[N:9]=[C:10]([CH3:11])[O:12][CH:13]=1)=[O:5])[CH3:2]参加物
5
反応条件
- 温度
- 110 °C
実験手順
5 g (25 mmol) of potassium 2-ethoxycarbonyl-2-(1-ethoxy-ethylideneamino)-ethenolate were completely dissolved in 15 mL acetic acid at RT, and then the solution was heated to 110° C. overnight. After cooling down, 100 mL EtOAc were added and the solution is neutralized with saturated NaHCO3 solution. The organic phase was separated, dried over Na2SO4, filtered and evaporated. Column chromatography on silica gel (heptane/EtOAc 1:2) yielded 1.74 g (45%) of 2-methyl-oxazole-4-carboxylic acid ethyl ester as an yellow oil, MS: 156 (MH+).
後処理
- temperatureAfter cooling down
- customThe organic phase was separated
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-c04230959fd24adb8c67e3a051985410
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07906546B2
反応ノート
読み込み中…