Sodium Hydroxide → 3-(4-Chlorophenyl)-4,5-dihydro-1H-pyrazole
反応式
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=O)[CH2:10][CH2:11][N:12](C)C)=[CH:5][CH:4]=1.O.[NH2:17]N.[OH-].[Na+]>CO>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:10][CH2:11][NH:12][N:17]=2)=[CH:5][CH:4]=1参加物
5
反応条件
- 温度
- 50 °C
実験手順
Under N2 atmosphere, 1-(4-chloro-phenyl)-3-dimethylamino-propan-1-one hydrochloride (37.2 g) was dissolved in warm MeOH (75 mL), and slowly added to a solution of hydrazine hydrate (23 mL) and 50% aqueous NaOH (12 mL) in MeOH (30 mL) stirred at 50° C. The mixture was refluxed for 2 hours, and evaporated under reduced pressure. Water was added to the residue, followed by extraction with DCM. The organic phase was washed twice with water, dried and evaporated under reduced pressure, to give 25.0 g of a yellow solid, m.p. 90-100° C.
後処理
- temperatureThe mixture was refluxed for 2 hours
- customevaporated under reduced pressure
- additionWater was added to the residue
- extractionfollowed by extraction with DCM
- washThe organic phase was washed twice with water
- customdried
- customevaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-92c5b61e2c3a4d50b6f5137860c46781
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08722887B2
反応ノート
読み込み中…