Hydrochloric Acid → (2-Fluorobenzyl)hydrazine dihydrochloride
反応式
[ClH:1].[F:2][C:3]1[CH:21]=[CH:20][CH:19]=[CH:18][C:4]=1[CH2:5][N:6](C(OC(C)(C)C)=O)[N:7]=C(C)C>C1COCC1>[ClH:1].[ClH:1].[F:2][C:3]1[CH:21]=[CH:20][CH:19]=[CH:18][C:4]=1[CH2:5][NH:6][NH2:7]参加物
4
実験手順
Aqueous hydrochloric acid (3 M, 60.64 mL, 181.92 mmol)I was added to a solution of tert-butyl 1-(2-fluorobenzyl)-2-isopropylidenehydrazinecarboxylate (17 g, 60.64 mmol) in THF (100 mL) and the mixture was heated at reflux for 3 h and concentrated. The residue was taken up in toluene and concentrated, then ether was added to the residue and the suspension was stirred for 30 min and filtered. The filter cake (12.2 g, 94%) was washed with ether and dried on the high vacuum pump. LC-MS [M-2HCl]=141.0, RT=0.25 min.
後処理
- temperaturethe mixture was heated
- temperatureat reflux for 3 h
- concentrationconcentrated
- concentrationconcentrated
- additionether was added to the residue
- filtrationfiltered
- washThe filter cake (12.2 g, 94%) was washed with ether
- customdried on the high vacuum pump
出典と根拠
- ORDレコード
- ord-70184066877e404487e34e290e25d121
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08431695B2
反応ノート
読み込み中…