Iodine → HCID 178509534、化合物
反応式
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([C:10]#[N:11])=[CH:7][CH:8]=2)[CH:3]=[N:2]1.[OH-].[K+].[I:14]I>CN(C=O)C>[I:14][C:3]1[C:4]2[C:9](=[CH:8][CH:7]=[C:6]([C:10]#[N:11])[CH:5]=2)[NH:1][N:2]=1参加物
5
実験手順
In a 25 ml round-bottomed flask, 1H-indazole-5-carbonitrile (400 mg, 2.79 mmol) was dissolved in DMF (7 ml). Potassium hydroxide (607 mg, 10.8 mmol) was added followed by iodine (1.42 g, 5.59 mmol). The dark brown suspension was stirred at room temperature for 3 h then was quenched with 10% aqueous NaHSO3 and extracted with diethyl ether (2×). The combined organic layers were washed twice with water and once with brine then dried over sodium sulfate, filtered and concentrated to give 396 mg (53%) of 3-iodo-1H-indazole-5-carbonitrile as a light yellow powder.
後処理
- customthen was quenched with 10% aqueous NaHSO3
- extractionextracted with diethyl ether (2×)
- washThe combined organic layers were washed twice with water and once with brine
- dry with materialthen dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-c2b291e73e01467881b4b5381f73f74f
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658646B2
反応ノート
読み込み中…