Bromine → (4-Bromo-2,3-dimethylphenyl)(methyl)sulfane
반응식
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[S:9][CH3:10].[Br:11]Br>C(O)(=O)C>[CH3:8][C:7]1[C:2]([CH3:1])=[C:3]([S:9][CH3:10])[CH:4]=[CH:5][C:6]=1[Br:11]참가 물질
4
실험 절차
510 g (3.33 mol) of 2,3-dimethylthioanisole are initially charged in 3 l of glacial acetic acid, and a solution of 592 g (7.4 mol) of bromine in 1 l of glacial acetic acid is added dropwise at room temperature over a period of three hours. The reaction is slightly exothermic. The reaction mixture is stirred at room temperature for another 3.5 hours. The precipitate is then filtered off with suction and the filtrate is admixed with 270 g of sodium acetate and concentrated. The residue is taken up in 2 l of dichloromethane and washed twice with 2 l of sodium bicarbonate solution and twice with sodium chloride solution. The organic phase is dried over sodium sulfate and concentrated.
후처리
- filtrationThe precipitate is then filtered off with suction
- concentrationconcentrated
- washwashed twice with 2 l of sodium bicarbonate solution and twice with sodium chloride solution
- dry with materialThe organic phase is dried over sodium sulfate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-a87ccfffb570475bb5d1517393d2a26a
- 출처 데이터셋
- uspto-grants-2003_12
- 특허 번호
- US06670482B2
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