反応式
[CH3:1][NH:2][C:3]1[CH2:7][O:6][C:5](=[O:8])[CH:4]=1.[OH-].[Na+].[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([CH2:18]Cl)=[CH:14][N:13]=1>C(COC)OC>[Cl:11][C:12]1[N:13]=[CH:14][C:15]([CH2:18][N:2]([CH3:1])[C:3]2[CH2:7][O:6][C:5](=[O:8])[CH:4]=2)=[CH:16][CH:17]=1参加物
5
反応条件
- 温度
- 50 °C
実験手順
30 g of 4-(methylamino)furan-2(5H)-one (Example 11) are initially charged in 450 ml of dimethoxyethane at room temperature. Subsequently, 12.6 g of sodium hydroxide are added and, at 40° C., 225 g of a 20% solution of 2-chloro-5-(chloromethyl)pyridine in dimethoxyethane are metered in. The mixture is stirred at 50° C. for a further 6 h. The solvent is substantially removed under reduced pressure and the residue is admixed with 300 ml of water. The solids are filtered off, washed with 150 ml of water and dried under reduced pressure. 58.7 g of 4-([[6-chloropyridin-3-yl]methyl](methy)amino)furan-2(5H)-one are obtained with a purity of 94% (this corresponds to 87% yield).
後処理
- customThe solvent is substantially removed under reduced pressure
- filtrationThe solids are filtered off
- washwashed with 150 ml of water
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-8236c195a16443edb1720bb9f06d759e
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08487112B2
関連ノート
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