3,4-Dimethylaniline → Glycine, N-(3,4-dimethylphenyl)-, methyl ester
反応式
[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]=1参加物
4
実験手順
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°.
後処理
- customThe cooled reaction mixture
- filtrationfiltered
- washThe collected solid was washed with ether (2×100 ml)
- concentrationthe combined filtrates were concentrated
出典と根拠
- ORDレコード
- ord-35c8639a29f5497781a5ef5fc97bc126
- 出典データセット
- uspto-grants-1991_01
- 特許番号
- US04985427
反応ノート
読み込み中…