N-bromobutanimide → HCID 67148260, 화합물

HRID 2426266노트

반응식

HRID 2426266 반응식
[C:1]([O:9][C:10]1[C:20](=[O:21])[N:14]2[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:13]2=[N:12][C:11]=1[C:22]([O:24][CH3:25])=[O:23])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Br:26]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[C:1]([O:9][C:10]1[C:20](=[O:21])[N:14]2[CH2:15][CH2:16][CH2:17][CH2:18][CH:19]([Br:26])[C:13]2=[N:12][C:11]=1[C:22]([O:24][CH3:25])=[O:23])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 67147764HCID 67147764, 화합물

생성물 1

HCID 67148260HCID 67148260, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

A mixture of methyl 3-(benzoyloxy)-4-oxo-4,6,7,8,9,10-hexahydropyrimido[1,2-a]azepine-2-carboxylate, N-bromo-succinimide (2 eq.) and α,α′-azoisobutyronitrile (0.45 eq.) in carbon tetrachloride was stirred under reflux for 14 hour. The mixture was cooled to room temperature, the succinimide was filtered off and the solvent was removed under reduced pressure. Methyl 3-(benzoyloxy)-10-bromo-4-oxo-4,6,7,8,9,10-hexahydropyrimido[1,2-a]azepine-2-carboxylate was obtained after flash chromatography (eluents petroleum ether/ethyl acetate, 8:2) as a pale yellow solid.

후처리

  1. temperatureunder reflux for 14 hour
  2. filtrationthe succinimide was filtered off
  3. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-3a6e79591a784a7fb1906d8698bb590f
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07968553B2

반응 노트

불러오는 중…