2-Methylbenzoxazole → 2-(Benzo[d]oxazol-2-yl)-N,N-dimethylethenamine
反応式
[CH3:1][C:2]1[O:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.C[C:12]([N:14]([CH3:16])[CH3:15])=O>CN(C=O)C>[O:3]1[C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=[C:2]1/[CH:1]=[CH:12]/[N:14]([CH3:16])[CH3:15]参加物
4
反応条件
- 温度
- 145 °C
実験手順
A mixture of 2-methylbenzo[d]oxazole (3 g, 22.6 mmol) in DMF (3.2 g) and dimethyl acetamide (3.5 g, 29.3 mmol) was stirred under N2 at 145° C. overnight. Then the solution was poured into ice-water and extracted with EtOAc (100 mL×2). The organic phase was washed, dried and concentrated. The residue was purified by column chromatography to get the title compound (2.2 g). MS (ESI) m/z 134 (M+H+).
後処理
- extractionextracted with EtOAc (100 mL×2)
- washThe organic phase was washed
- customdried
- concentrationconcentrated
- customThe residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-8751eac5577644d588bc9396371a866f
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969349B2
反応ノート
読み込み中…