N-bromobutanimide → HCID 23298010、化合物

HRID 1422210ノート

反応式

HRID 1422210 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 23298010HCID 23298010、化合物

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-94c68e858ea046f886de8dc83e034cfe
出典データセット
uspto-grants-2000_06
特許番号
US06080743

反応ノート

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