반응식
[Br:1][C:2]1[CH:3]=[C:4]([N:8](C)[C:9](=O)OC(C)(C)C)[CH:5]=[CH:6][CH:7]=1.FC(F)(F)C(O)=O.C(=O)([O-])O.[Na+]>ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[NH:8][CH3:9]참가 물질
5
실험 절차
3.6 g (12.7 mmol) of tert-butyl (3-bromophenyl)-N-methylcarbamate, prepared in a manner analogous to Example 1b), are dissolved in 15 ml of dichloromethane. 5 ml of trifluoroacetic acid are added and the reaction mixture is stirred at ambient temperature for 1 hour. The reaction is halted by the addition of 50 ml of a saturated sodium hydrogencarbonate solution and then extraction is carried out with ethyl acetate. The organic phases are combined and dried over sodium sulfate. The solvents are evaporated and then the residue is chromatographed on silica gel (heptane/ethyl acetate 50/50). 2.14 g of 3-bromo-N-methylaniline are obtained in the form of an oil. Yield=90%.
후처리
- extractionextraction
- dry with materialdried over sodium sulfate
- customThe solvents are evaporated
- customthe residue is chromatographed on silica gel (heptane/ethyl acetate 50/50)
출처 및 근거
- ORD 기록
- ord-c24b085d45fe4a24b8a82edbe47772a9
- 출처 데이터셋
- uspto-grants-2009_12
- 특허 번호
- US07626054B2
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