Ethyl orthoformate → 6-Tetrazol-1-yl-pyridin-3-ol
反応式
[N-:1]=[N+:2]=[N-:3].[Na+].C(OC([O:12][CH2:13][CH3:14])OCC)C.[NH2:15][C:16]1[N:21]=[CH:20]C(O)=[CH:18][CH:17]=1>CC(O)=O>[N:21]1([C:16]2[N:15]=[CH:14][C:13]([OH:12])=[CH:18][CH:17]=2)[CH:20]=[N:3][N:2]=[N:1]1参加物
5
反応条件
- 温度
- 100 °C
実験手順
NaN3 (2.89 g, 44 mmol) and triethylorthoformate (7.4 ml, 44 mmol) were added to commercially available 6-amino-pyridin-3-ol (3.5 g, 32 mmol) in AcOH (50 mL). The reaction mixture was heated to 100° C. for 1-3 hours. The reaction was cooled to room temperature and left to stand overnight. The precipitate was filtered, washed with EtOAc (150 mL) and dried in vacuo. The crude product was obtained as a beige solid and used in the next step without further purification.
後処理
- temperatureThe reaction was cooled to room temperature
- waitleft
- filtrationThe precipitate was filtered
- washwashed with EtOAc (150 mL)
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-e334b9dea03d4ab796ae954b007b83a0
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08183381B2
反応ノート
読み込み中…