Hydrochloric Acid → 1-(2,5-Difluorophenyl)-1H-pyrazole
반응식
CO[CH:3](OC)[CH2:4][CH:5](OC)OC.[F:12][C:13]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=1[NH:20][NH2:21].Cl>C(O)C>[F:12][C:13]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=1[N:20]1[CH:5]=[CH:4][CH:3]=[N:21]1참가 물질
5
실험 절차
Add 1,1,3,3-tetramethoxypropane (8.2 g, 50 mmol) to a mixture of 2,5-difluorophenylhydrazine (9.022 g, 62.6 mmol) and hydrochloric acid (5M, 5 mL, 25 mmol) in ethanol (50 mL) and heat and stir under reflux under nitrogen for 17 hr. Cool the mixture, evaporate the ethanol in vacuo, suspend the residue in DCM (80 mL), filter the DCM solution and pass through an SCX-2 column. Collect the eluent and pass through a second SCX2 column and evaporate the eluent to give 1-(2,5-difluoro-phenyl)-1H-pyrazol as a liquid (8.79 g, 97%). MS (m/z): 181 (M+1).
후처리
- temperatureheat
- temperatureunder reflux under nitrogen for 17 hr
- temperatureCool the mixture
- customevaporate the ethanol in vacuo
- filtrationfilter the DCM solution and pass through an SCX-2 column
- customCollect the eluent
- customevaporate the eluent
출처 및 근거
- ORD 기록
- ord-66b657553e3f4520b9978e0d95e629ba
- 출처 데이터셋
- uspto-grants-2011_03
- 특허 번호
- US07910588B2
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