Water → HCID 178419467、化合物
反応式
[Br:1][C:2]1[C:3](O)=[N:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.O.[NH2:14][NH2:15].Cl.Cl.NN.O>C(O)CO>[Br:1][C:2]1[C:3]([NH:4][C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=2)=[N:14][NH:15][CH:11]=1参加物
6
実験手順
The bromohydroxyquinoline (1.97 g, 8.79 mmol) was dissolved in 21 ml of ethylene glycol and hydrazine hydrat (4.2 ml) was added. To this mixture were added 1.3 g (12.2 mmol) of hydrazine dihydrochloride, and the resulting mixture was heated to reflux and stirred under nitrogen. The resulting material was poured onto 300 ml of H2O. The mixture was extracted with CH2Cl2, basified with NaHCO3 and extracted further with CH2Cl2. The combined organic portions were washed with water, dried over Na2SO4, filtered, and concentrated in vacuo to give a brown oil, yielding bromoanilinopyrazole (i.e., 3-(2-amino-5-bromophenyl)pyrazole).
後処理
- temperaturethe resulting mixture was heated
- temperatureto reflux
- extractionThe mixture was extracted with CH2Cl2
- extractionextracted further with CH2Cl2
- washThe combined organic portions were washed with water
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give a brown oil
出典と根拠
- ORDレコード
- ord-f214bc5bf69247e5a3a8f05209bf673b
- 出典データセット
- uspto-grants-1992_10
- 特許番号
- US05153196
反応ノート
読み込み中…