Hydrochloric Acid → 1-(2,5-Difluorophenyl)-1H-pyrazole
反応式
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]1参加物
5
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-66b657553e3f4520b9978e0d95e629ba
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07910588B2
反応ノート
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