反応式
[OH:1][CH2:2][CH2:3][CH2:4][N:5]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[C:8](=[O:15])[NH:7][C:6]1=[O:16].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.CCOCC>C1COCC1>[F:13][C:11]([F:12])([F:14])[C:9]1[C:8](=[O:15])[NH:7][C:6](=[O:16])[N:5]([CH2:4][CH2:3][CH:2]=[O:1])[CH:10]=1参加物
5
反応条件
- 温度
- 0 °C
実験手順
1-(3-Hydroxy-propyl)-5-trifluoromethyl-1H-pyrimidine-2,4-dione (Prep20, 100 mg, 0.42 mmol) was dissolved in dry THF (5 mL), the solution was then cooled to 0° C. and Dess-Martin periodinane (300 mg, 0.71 mmol) was added. The mixture was stirred at 0° C. for 1.5 hours. Et2O was added and the mixture washed with aqueous saturated NaHCO3 solution. The organic phase was dried (Na2SO4) and evaporated. The crude was purified by flash chromatography with ethyl acetate-petroleum ether (1-1) to give 50 mg of title compound (68% yield).
後処理
- washthe mixture washed with aqueous saturated NaHCO3 solution
- dry with materialThe organic phase was dried (Na2SO4)
- customevaporated
- customThe crude was purified by flash chromatography with ethyl acetate-petroleum ether (1-1)
出典と根拠
- ORDレコード
- ord-7803cddafcb04961b30e4533461f82af
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07727988B2
関連ノート
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