Bromine → HCID 15718183、化合物

HRID 982361ノート

反応式

HRID 982361 の反応式
[C:1]([C:4]1[N:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]2=[N:6][CH:5]=1)(=[O:3])[CH3:2].[BrH:13].C(O)(=O)C.BrBr>C(O)(=O)C>[Br:13][CH2:2][C:1]([C:4]1[N:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]2=[N:6][CH:5]=1)=[O:3]

参加物

5

反応物 3

HCID 24408BromineHCID 157181821-(Imidazo[1,2-a]pyridin-3-yl)ethan-1-oneHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

生成物 1

HCID 15718183HCID 15718183、化合物収率 40%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
40 °C

実験手順

22.1 g of 3-acetylimidazo[1,2-a]pyridine was dissolved in 220 ml of acetic acid. 35.1 ml of a 30% hydrogen bromide/acetic acid solution was added dropwise to the solution at 0° C. Then 28.6 g of bromine was added dropwise thereto at 40° C. The mixture was stirred at 40° C. for 2 h and crystals thus formed were filtered. The crystals were dissolved in 100 ml of water. The solution was made alkaline with an excess of an aqueous sodium hydrogencarbonate solution and then extracted with ethyl acetate. The organic layer was concentrated and the obtained brown solid was purified according to silica gel column chromatography (eluted with ethyl acetate) to obtain 13.5 g (yield: 40%) of 3-bromoacetylimidazo[1,2-a]pyridine (yield: 40%) in the form of yellow crystals.

後処理

  1. customat 40° C
  2. customcrystals thus formed
  3. filtrationwere filtered
  4. dissolutionThe crystals were dissolved in 100 ml of water
  5. extractionextracted with ethyl acetate
  6. concentrationThe organic layer was concentrated
  7. customthe obtained brown solid was purified
  8. washaccording to silica gel column chromatography (eluted with ethyl acetate)

出典と根拠

ORDレコード
ord-517b720b359541f98cc401b5169b3e4a
出典データセット
uspto-grants-1991_02
特許番号
US04996215

反応ノート

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