反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([CH3:12])[CH:3]=1.COCC(O)C.[N:19]1([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1>>[CH3:12][C:4]1[CH:3]=[C:2]([N:22]2[CH2:21][CH2:20][N:19]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:24][CH2:23]2)[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1参加物
4
実験手順
4-Chloro-2-methylquinoline (5 g, 28 mmol) was mixed with 1-methoxy-2-propanol, tert-butyl piperazine-1-carboxylate was added (5.74 g, 30.8 mmol) and the mixture was refluxed for 4.5 hours after which the product started to precipitate. The mixture was concentrated under reduced pressure and left at room temperature for 48 hours. The product was separated by filtration, washed with ethylacetate and dried at 50° C. 4.382 g of a solid were obtained (13.38 mmol, 48%). MS (APCI): m/z=327.9 [M+1]+.
後処理
- additionwas added (5.74 g, 30.8 mmol)
- temperaturethe mixture was refluxed for 4.5 hours after which the product
- customto precipitate
- concentrationThe mixture was concentrated under reduced pressure
- customThe product was separated by filtration
- washwashed with ethylacetate
- customdried at 50° C
出典と根拠
- ORDレコード
- ord-183f7a13eb6341c1a117023f1fbe0cec
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08883791B2
関連ノート
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