反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([S:8][CH3:9])[C:3]=1[C:10]1[CH2:14][CH2:13][O:12][N:11]=1.[Br:15]Br>S(=O)(=O)(O)O>[Br:15][C:7]1[C:2]([CH3:1])=[C:3]([C:10]2[CH2:14][CH2:13][O:12][N:11]=2)[C:4]([S:8][CH3:9])=[CH:5][CH:6]=1参加物
実験手順
At 0° C., 10 g (48 mmol) of 3-(2-methyl-6-methylthiophenyl)-4,5-dihydroisoxazole are added a little at a time to 120 ml of conc. sulfuric acid, and the mixture is stirred for approximately 30 minutes. 3.7 g (23 mmol) of bromine are then added dropwise, and the mixture is stirred at 0° C. for 2.5 hours. Over a period of approximately 45 minutes, the mixture is subsequently allowed to warm to room temperature. A homogeneous solution forms. For work-up, the reaction mixture is poured into ice-water and extracted three times with methylene chloride. The organic phase is washed with sodium bicarbonate solution, dried with magnesium sulfate and concentrated. This gives 11.4 g of crude product which is employed in the next step without any further purification.
後処理
- stirringthe mixture is stirred at 0° C. for 2.5 hours
- waitOver a period of approximately 45 minutes
- extractionextracted three times with methylene chloride
- washThe organic phase is washed with sodium bicarbonate solution
- dry with materialdried with magnesium sulfate
- concentrationconcentrated
- customThis gives 11.4 g of crude product which is employed in the next step without any further purification
出典と根拠
- ORDレコード
- ord-29d7ae22d20b492fab7f05477303e742
- 出典データセット
- uspto-grants-2003_12
- 特許番号
- US06670482B2
関連ノート
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