3,4-Dimethylaniline → Glycine, N-(3,4-dimethylphenyl)-, methyl ester
반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[CH3:9])[NH2:5].Br[CH2:11][C:12]([O:14][CH3:15])=[O:13]>CCOCC>[CH3:15][O:14][C:12](=[O:13])[CH2:11][NH:5][C:4]1[CH:6]=[CH:7][C:8]([CH3:9])=[C:2]([CH3:1])[CH:3]=1참가 물질
4
실험 절차
3,4-Dimethylaniline (70.0 g) and methyl bromoacetate (44.2 g) were stirred at 100° under nitrogen for 2 h. The cooled reaction mixture was poured into ether (700 ml) and filtered. The collected solid was washed with ether (2×100 ml) and the combined filtrates were concentrated to give a solid (45.6 g) which was purified by FCC on triethylamine deactivated silica eluting with dichloromethane: petroleum ether (1:3) to give a solid (21.8 g), a portion of which (2.5 g) was purified further by FCC as above to give the title compound (2.06 g), m.p. 53°-55°.
후처리
- customThe cooled reaction mixture
- filtrationfiltered
- washThe collected solid was washed with ether (2×100 ml)
- concentrationthe combined filtrates were concentrated
출처 및 근거
- ORD 기록
- ord-58ba0cd2165e4ad8a7520ae19361556f
- 출처 데이터셋
- uspto-grants-1991_06
- 특허 번호
- US05023255
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