反応式
CN(C)C=O.CS([C:10]1[N:15]=[C:14]([CH3:16])[C:13]([C:17]([O:19][CH2:20][CH2:21][C:22]([CH3:26])=[C:23]([F:25])[F:24])=[O:18])=[CH:12][N:11]=1)(=O)=O.[CH2:27]([NH:31][CH3:32])[CH2:28][CH2:29][CH3:30]>O>[CH2:27]([N:31]([C:10]1[N:15]=[C:14]([CH3:16])[C:13]([C:17]([O:19][CH2:20][CH2:21][C:22]([CH3:26])=[C:23]([F:25])[F:24])=[O:18])=[CH:12][N:11]=1)[CH3:32])[CH2:28][CH2:29][CH3:30]参加物
実験手順
To 3 ml of N,N-dimethylformamide were dissolved 0.50 g (1.6 mmol) of 4,4-difluoro-3-methyl-3-butenyl 2-methanesulfonyl-4-methylpyrimidine-5-carboxylate, followed by the addition of 0.28 g (3.2 mmol) of N-butyl-N-methylamine and stirring at room temperature for 30 minutes. The reaction liquid was then poured in water and extracted with diethyl ether. 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 ether:hexane=1:7) to obtain 0.41 g (yield: 80%) of 4,4-difluoro-3-methyl-3-butenyl 2-(N-butyl-N-methylamino)-4-methylpyrimidine-5-carboxylate.
後処理
- customThe reaction liquid
- extractionextracted with diethyl ether
- 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 ether:hexane=1:7)
出典と根拠
- ORDレコード
- ord-902c14b103ff4726a2055043bd4326fe
- 出典データセット
- uspto-grants-2007_09
- 特許番号
- US07273878B2
関連ノート
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