4Iodo-benzoic acid N'-(2,2-dimethyl-propionyl)-hydrazide → 4-Iodobenzenecarbohydrazide
反応式
CC(C)(C)C([NH:5][NH:6][C:7](=[O:15])[C:8]1[CH:13]=[CH:12][C:11]([I:14])=[CH:10][CH:9]=1)=O>FC(F)(F)C(O)=O>[I:14][C:11]1[CH:12]=[CH:13][C:8]([C:7]([NH:6][NH2:5])=[O:15])=[CH:9][CH:10]=1参加物
3
実験手順
Trifluoroacetic acid (10 ml) was added to 4iodo-benzoic acid N′-(2,2-dimethyl-propionyl)-hydrazide (Intermediate 13) (1 g, 2.76 mmol) and stirred at room temperature for 2 hours. The trifluoroactic acid was removed in vacuo and the residue partitioned between ethyl acetate (50 ml) and saturated aqueous sodium bicarbonate solution (50 ml). The organic layer was washed with water (50 ml), brine (50 ml), dried over magnesium sulfate, filtered and the solvent removed in vacuo. The desired product was obtained as a white solid (0.55 g, 2.1 mmol).
後処理
- customThe trifluoroactic acid was removed in vacuo
- customthe residue partitioned between ethyl acetate (50 ml) and saturated aqueous sodium bicarbonate solution (50 ml)
- washThe organic layer was washed with water (50 ml), brine (50 ml)
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customthe solvent removed in vacuo
出典と根拠
- ORDレコード
- ord-ac02ab09da504815b72b4796a3df3564
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07425555B2
反応ノート
読み込み中…