Chlorosuccinimide → 2-chloro-N,N-dimethyl-3-nitro-aniline
반응식
[CH3:1][N:2]([CH3:12])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N+:9]([O-:11])=[O:10])[CH:4]=1.[Cl:13]N1C(=O)CCC1=O>CN(C=O)C>[CH3:1][N:2]([CH3:12])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N+:9]([O-:11])=[O:10])[C:4]=1[Cl:13]참가 물질
4
실험 절차
25 g of N,N-dimethyl-3-nitroaniline is dissolved in 225 ml of DMF. 20 g of N-chlorosuccinimide dissolved in 190 ml of DMF is slowly added dropwise and the solution is stirred at RT. After 24 hours, the solvent is evaporated. About 500 ml of ice is added to the red residue. The suspension is extracted three times with about 200 ml of diethylether. The ether phases are dried over Na2SO4, filtered, and evaporated down. 30.4 g of N,N-dimethyl-2-chloro-3-nitroaniline is obtained as a red oil. The crude product is used further without any additional purification.
후처리
- additionis slowly added dropwise
- customthe solvent is evaporated
- additionAbout 500 ml of ice is added to the red residue
- extractionThe suspension is extracted three times with about 200 ml of diethylether
- dry with materialThe ether phases are dried over Na2SO4
- filtrationfiltered
- customevaporated down
출처 및 근거
- ORD 기록
- ord-6ec2464b864f4df392236929417f9e8e
- 출처 데이터셋
- uspto-grants-2004_06
- 특허 번호
- US06747051B2
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