Formic Acid → 1,3-Benzoxazole-4-carboxylic acid
反応式
[NH2:1][C:2]1[C:10](N)=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH:12](O)=[O:13]>Cl>[O:13]1[C:10]2=[CH:9][CH:8]=[CH:7][C:3]([C:4]([OH:6])=[O:5])=[C:2]2[N:1]=[CH:12]1参加物
4
実験手順
A mixture of 2,3-diaminobenzoic acid (0.5 g, 3.29 mmol) and formic acid (405 μl, 9.87 mmol) in hydrochloric acid (4M, 10 ml) was heated under reflux for one hour. The precipitate which formed on cooling was collected, redissolved in boiling methanol, and decolorised with activated charcoal. Evaporation of the solvent gave benzoxazole-4-carboxylic acid as a white powder (407.9 mg, 77%) Found: C, 46.11; H, 3.63; N, 13.27. C8H6N2O2.HCl.0.5 H2O requires C, 46.28; H, 3.88; N, 13.49%; δH (d6-DMSO, 200 MHz) 7.7-7.8; (1H, t, Ar-5H), 8.2-8.3 (2H, dd, Ar-4/6H), 9.65 (1H, s, imidazole-2H).
後処理
- temperaturewas heated
- temperatureunder reflux for one hour
- customThe precipitate which formed
- temperatureon cooling
- customwas collected
- dissolutionredissolved
- customEvaporation of the solvent
出典と根拠
- ORDレコード
- ord-3eee5a06d86045f5a2db757251c83abd
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06310082B1
反応ノート
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