反応式
CN(C)C=O.CS([O:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]([CH3:19])=[C:16]([F:18])[F:17])(=O)=O.[CH3:20][C:21]1[N:22]=[C:23]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[S:24][C:25]=1[C:26](O)=[O:27].C(=O)([O-])O.[Na+]>O>[CH3:20][C:21]1[N:22]=[C:23]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[S:24][C:25]=1[C:26]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]([CH3:19])=[C:16]([F:17])[F:18])=[O:27]参加物
反応条件
- 温度
- 100 °C
実験手順
To 10 ml of N,N-dimethylformamide were dissolved 0.50 g (2.2 mmol) of 6,6-difluoro-5-methyl-5-hexenyl methanesulfonate and 0.53 g (2.4 mmol) of 4-methyl-2-phenylthiazole-5-carboxylic acid, followed by the addition of 0.37 g (4.4 mmol) of sodium hydrogencarbonate and stirring at 100° C. for 6 hours. The reaction liquid was then poured in water and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentration under reduced pressure. The residue was purified with silica gel column chromatography (ethyl acetate:hexane=1:19) to obtain 0.57 g (yield: 74%) of 6,6-difluoro-5-methyl-5-hexenyl 4-methyl-2-phenylthiazole-5-carboxylate.
後処理
- customThe reaction liquid
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materialby drying over anhydrous magnesium sulfate and concentration under reduced pressure
- customThe residue was purified with silica gel column chromatography (ethyl acetate:hexane=1:19)
出典と根拠
- ORDレコード
- ord-ed3a289d1c7047d889f544ad0741d157
- 出典データセット
- uspto-grants-2007_09
- 特許番号
- US07273878B2
関連ノート
読み込み中…