Trimethyl orthoformate → 1,3-Benzoxazole-7-carboxylic acid
反応式
[NH2:1][C:2]1[C:3]([OH:11])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].[CH:12](OC)(OC)OC>>[O:11]1[C:3]2[C:4]([C:5]([OH:7])=[O:6])=[CH:8][CH:9]=[CH:10][C:2]=2[N:1]=[CH:12]1参加物
3
実験手順
A solution of 3-amino-2-hydroxy-benzoic acid (12.5 mmol) in trimethyl orthoformate (19.2 mL) is heated to reflux for 20 h and concentrated in vacuo. The residue is washed three times with hot MeOH, the filtrates are combined and the solvent is removed in vacuo to give the desired product which is used without further purification. 1H-NMR (DMSO-d6): δ=13.4 (bs, 1H); 8.87 (s, 1H); 8.08 (d, J=8.0 Hz, 1H); 7.96 (d, J=7.5 Hz, 1H); 7.52 (t, J=7.9 Hz, 1H).
後処理
- temperatureto reflux for 20 h
- concentrationconcentrated in vacuo
- washThe residue is washed three times with hot MeOH
- customthe solvent is removed in vacuo
出典と根拠
- ORDレコード
- ord-eb43d318344b4462a94fa34419a801f6
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063099B2
反応ノート
読み込み中…