N-bromobutanimide → HCID 58459174, 화합물

HRID 2036560노트

반응식

HRID 2036560 반응식
[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]

참가 물질

4

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1db06fb30cba41d0b17537fe0ff298fe
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08575183B2

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