반응식
C(NC(OC1C=C(C(=O)C[Br:21])C=C(OC(=O)NCC)C=1)=O)C.[CH2:23]([NH:30][C:31]([CH3:34])([CH3:33])[CH3:32])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>CC(C)=O>[BrH:21].[CH2:23]([NH:30][C:31]([CH3:34])([CH3:33])[CH3:32])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1참가 물질
4
실험 절차
To a solution of 8.0 g of 3',5'-bis-(N-ethylcarbamoyloxy)-2-bromo acetophenone in 100 ml of acetone was added 7.0 g of N-benzyl-t-butylamine. The mixture was refluxed for 18 hours. The 4.1 g of N-benzyl-t-butylamine hydrobromide formed and precipitated during the reaction was filtered off and the filtrate was acidified with conc. HCl. The filtrate was now evaporated to dryness and the title compound was isolated by column chromatography on Silica gel 60 using (1) CHCl3 /ethanol (2:1), (2) ethanol as eluants. The title compound was eluted in the ethanol fraction and recrystallized from ethanol/diethylether. The identity of the product was confirmed with NMR.
후처리
- temperatureThe mixture was refluxed for 18 hours
출처 및 근거
- ORD 기록
- ord-7fe92459100740a0b008c2a568a04930
- 출처 데이터셋
- uspto-grants-1984_05
- 특허 번호
- US04451663
연결된 노트
불러오는 중…