反応式
[C:1]([O:7][CH2:8][CH3:9])(=[O:6])[CH2:2][C:3]([CH3:5])=O.[CH3:10]OC(OC)N(C)C.Cl.[C:19]1([NH:25][NH2:26])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C(O)C>[CH3:5][C:3]1[N:25]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[N:26]=[CH:10][C:2]=1[C:1]([O:7][CH2:8][CH3:9])=[O:6]参加物
5
反応条件
- 温度
- 120 °C
実験手順
A mixture of ethyl acetoacetate (1.5 g, 11.5 mmol) and dimethylformamide dimethyl acetal (1.68 mL, 12.7 mmol) was stirred at 120° C. for 2 hours. The reaction solution was cooled to room temperature, and a solution of phenyl hydrazine hydrochloride (1.67 g, 11.5 mmol) in ethanol (30 mL) was then added thereto. The obtained mixture was stirred at 80° C. for 2.5 hours. The reaction solution was cooled to room temperature, and it was then concentrated under reduced pressure. The residue was purified with a fractionation purification apparatus (Biotage, ethyl acetate:hexane=1:19-3:7), so as to obtain the title compound (2.32 g, 87%) in the form of a yellow oily product.
後処理
- temperatureThe reaction solution was cooled to room temperature
- stirringThe obtained mixture was stirred at 80° C. for 2.5 hours
- temperatureThe reaction solution was cooled to room temperature
- concentrationit was then concentrated under reduced pressure
- customThe residue was purified with a fractionation purification apparatus (Biotage, ethyl acetate:hexane=1:19-3:7)
出典と根拠
- ORDレコード
- ord-56649bbc9a974d688e5688716682c800
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08648103B2
関連ノート
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