N-bromobutanimide → HCID 23298010, 화합물

HRID 1422210노트

반응식

HRID 1422210 반응식
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[N:9]2)=[C:4]([CH3:16])[CH:3]=1.[Br:17]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[N:9]2)=[C:4]([CH2:16][Br:17])[CH:3]=1

참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 232980507-Bromo-5-methyl-2,3-dimethoxy-quinoxaline

생성물 1

HCID 23298010HCID 23298010, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

15 g (53 mmol) of 7-bromo-5-methyl-2,3-dimethoxy-quinoxaline, 9.9 g (1.05 equiv.) of N-bromosuccinimide and 0.87 g (0.1 equiv.) of azo-isobutyronitrile are dissolved in 100 ml of carbon tetrachloride and the solution is stirred at reflux for 24 hours. The solid is filtered off and the filtrate is diluted with dichloromethane, then washed once with each of water and brine. The organic phase is dried over magnesium sulfate and concentrated by evaporation. The residue is recrystallized from ethyl acetate and hexane. The title compound is obtained in the form of light-orange crystals.

후처리

  1. temperatureat reflux for 24 hours
  2. filtrationThe solid is filtered off
  3. additionthe filtrate is diluted with dichloromethane
  4. washwashed once with each of water and brine
  5. dry with materialThe organic phase is dried over magnesium sulfate
  6. concentrationconcentrated by evaporation
  7. customThe residue is recrystallized from ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-94c68e858ea046f886de8dc83e034cfe
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06080743

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