3-Bromo-1,1,1-trifluoro-2-propanone → Ethyl 4-(trifluoromethyl)thiazole-2-carboxylate
反応式
[NH2:1][C:2](=[S:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4].Br[CH2:10][C:11](=O)[C:12]([F:15])([F:14])[F:13]>C(O)C>[F:13][C:12]([F:15])([F:14])[C:11]1[N:1]=[C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])[S:8][CH:10]=1参加物
4
実験手順
A solution of ethyl amino(thioxo)acetate (4 g) and 3-bromo-1,1,1-trifluoroacetone (3.1 ml) in ethanol (150 ml) was heated under reflux overnight. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate) to give the title compound (3.56 g).
後処理
- temperatureunder reflux overnight
- concentrationThe reaction mixture was concentrated under reduced pressure
- additionthe residue was diluted with water
- extractionextracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe obtained residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate)
出典と根拠
- ORDレコード
- ord-952f4d1a092b4325a976f92b6c14a45f
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09199963B2
反応ノート
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