반응식
[CH2:1](Br)[C:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[O:3].[CH3:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([NH2:20])[CH:15]=1.C([O-])([O-])=O.[Na+].[Na+]>C(O)C>[CH2:12]([O:13][C:14]1[CH:15]=[C:16]([NH:20][C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:2](=[O:3])[CH3:1])[CH:17]=[CH:18][CH:19]=1)[CH3:11]참가 물질
5
실험 절차
5 g of phenacyl bromide and 3.78 g of m-phenetidine are stirred at 50° C. for 2.5 h in 50 ml of ethanol in the presence of 5.85 g of powdered Na2CO3. The mixture is then cooled and concentrated in an RE. The residue is partitioned between water and methylene chloride and the aqueous phase is extracted twice with methylene chloride. The combined organic phases are dried over Na2SO4 and concentrated. The residue is slurried with ether and the crystals are filtered off, 2'-(3-ethoxyphenylamino)acetophenone being obtained. Further product is again obtained from the mother liquor after addition of petroleum ether.
후처리
- temperatureThe mixture is then cooled
- concentrationconcentrated in an RE
- customThe residue is partitioned between water and methylene chloride
- extractionthe aqueous phase is extracted twice with methylene chloride
- dry with materialThe combined organic phases are dried over Na2SO4
- concentrationconcentrated
- filtrationthe crystals are filtered off
출처 및 근거
- ORD 기록
- ord-a4c2f8e276d2461884398f346404e01b
- 출처 데이터셋
- uspto-grants-1999_02
- 특허 번호
- US05869485
연결된 노트
불러오는 중…