N-bromobutanimide → HCID 58459174、化合物

HRID 2036560ノート

反応式

HRID 2036560 の反応式
[Cl:1][C:2]1[C:3]2[N:4]([CH:8]=[C:9]([CH2:11][Cl:12])[N:10]=2)[CH:5]=[CH:6][CH:7]=1.[Br:13]N1C(=O)CCC1=O>C(#N)C>[Br:13][C:8]1[N:4]2[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[C:3]2=[N:10][C:9]=1[CH2:11][Cl:12]

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 573552298-Chloro-2-(chloromethyl)imidazo[1,2-A]pyridine

生成物 1

HCID 58459174HCID 58459174、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Acetonitrile (8.5 ml) was added to 8-chloro-2-(chloromethyl)imidazo[1,2-a]-pyridine (341 mg, 1.7 mmol). N-bromosuccinimide (302 mg, 1.7 mL) was added and the mixture was stirred at rt until complete. The reaction mixture was partitioned with EtOAc and satd. aq. NaHCO3 solution. The organic layer was dried with Na2SO4, filtered, and concentrated under reduced pressure. The residue was taken up in DCM and purified by chromatography on a 23 g silica gel column using 0 to 70% gradient of EtOAc in hexane. The desired fractions were combined and concentrated under reduced pressure to give 3-bromo-8-chloro-2-(chloromethyl)imidazo[1,2-a]pyridine as a white crystalline solid.

後処理

  1. customThe reaction mixture was partitioned with EtOAc
  2. dry with materialThe organic layer was dried with Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. custompurified by chromatography on a 23 g silica gel column
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1db06fb30cba41d0b17537fe0ff298fe
出典データセット
uspto-grants-2013_11
特許番号
US08575183B2

反応ノート

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