反応式
[OH:1][C:2]1[CH2:6][O:5][C:4](=[O:7])[C:3]=1[C:8]([O:10]C)=O.[Cl:12][C:13]1[N:18]=[CH:17][C:16]([CH2:19][NH:20][CH2:21][CH:22]([F:24])[F:23])=[CH:15][CH:14]=1>C(#N)CCC>[Cl:12][C:13]1[N:18]=[CH:17][C:16]([CH2:19][N:20]([CH2:21][CH:22]([F:24])[F:23])[C:8]([C:3]2[C:4](=[O:7])[O:5][CH2:6][C:2]=2[OH:1])=[O:10])=[CH:15][CH:14]=1参加物
4
反応条件
- 温度
- 65 °C
実験手順
10 g of methyl 4-hydroxy-2-oxo-2,5-dihydrofuran-3-carboxylate are initially introduced in 111 g of butyronitrile and admixed with 5 g of N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethanamine. The solution is heated at 65° C. for 3 h. The solution is then extracted with 300 ml of water and then washed with 300 ml of 5% strength hydrochloric acid solution. The organic phase is dried over magnesium sulphate and the solvent is removed in vacuo. For purification, recrystallization from isopropanol is carried out.
後処理
- extractionThe solution is then extracted with 300 ml of water
- washwashed with 300 ml of 5% strength hydrochloric acid solution
- dry with materialThe organic phase is dried over magnesium sulphate
- customthe solvent is removed in vacuo
- customFor purification, recrystallization from isopropanol
出典と根拠
- ORDレコード
- ord-33b2f7e565e44cbd870ad14183a7eeae
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08680285B2
関連ノート
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