Methanol → HCID 178499646、化合物
反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH2:10][C:11]([OH:13])=[O:12])=[N:2]1.[CH3:14]O>S(=O)(=O)(O)O>[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH2:10][C:11]([O:13][CH3:14])=[O:12])=[N:2]1参加物
4
実験手順
A solution of 1H-indazole-3-acetic acid (1.0 g) prepared according to J. Am. Chem. Soc., 79, 5245 (1957), in methanol (30 ml) containing five drops of concentrated sulfuric acid was refluxed for 8 hours. The reaction mixture was then concentrated to a low volume and diluted with ethyl acetate (20 ml). The organic layer was washed with water (2×10 ml) and then with sodium bicarbonate solution (10 ml, 10%). The ethyl acetate layer was collected and then dried to obtain the title compound (yield: 0.8 g; m.p. 146° C.).
後処理
- temperaturewas refluxed for 8 hours
- concentrationThe reaction mixture was then concentrated to a low volume
- additiondiluted with ethyl acetate (20 ml)
- washThe organic layer was washed with water (2×10 ml)
- customThe ethyl acetate layer was collected
- customdried
出典と根拠
- ORDレコード
- ord-2faff251b83b4c28b4a5a1fdc5e04f27
- 出典データセット
- uspto-grants-1991_12
- 特許番号
- US05075442
反応ノート
読み込み中…