Hydrochloric Acid → (2-Fluorobenzyl)hydrazine dihydrochloride
반응식
[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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-70184066877e404487e34e290e25d121
- 출처 데이터셋
- uspto-grants-2013_04
- 특허 번호
- US08431695B2
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