Iodine → HCID 178506571、化合物
反応式
[NH:1]1[C:5]2[CH:6]=[CH:7][S:8][C:4]=2[CH:3]=[N:2]1.[I:9]I.[OH-].[K+].S(=O)(O)[O-].[Na+]>CN(C)C=O.O>[I:9][C:3]1[C:4]2[S:8][CH:7]=[CH:6][C:5]=2[NH:1][N:2]=1参加物
7
実験手順
To a solution of 1H-thieno[3,2-c]pyrazole (160 mg, 1.29 mmol) and iodine (490 mg, 1.94 mmol) in dimethyl formamide (5 mL) is added potassium hydroxide (220 mg, 3.87 mmol). The mixture is stirred at room temperature for 30 minutes. A solution of sodium bisulfite (200 mg) in water (2 mL) is then added. It is extracted twice with diethyl ether. The combined organic layers are dried over magnesium sulfate and concentrated. The residue is chromatographed (n-heptane-ethyl acetate, 90:100) to afford 195 mg (60%) of 3-iodo-1H-thieno[3,2-c]pyrazole as a beige powder. LC/MS: RT=2.50 minutes, 250.90 m/e (M+1).
後処理
- extractionIt is extracted twice with diethyl ether
- dry with materialThe combined organic layers are dried over magnesium sulfate
- concentrationconcentrated
- customThe residue is chromatographed (n-heptane-ethyl acetate, 90:100)
出典と根拠
- ORDレコード
- ord-d89c3474b7d24e108782ee5b82e3e880
- 出典データセット
- uspto-grants-2009_04
- 特許番号
- US07518000B2
反応ノート
読み込み中…