N-bromobutanimide → HCID 58531057, 화합물

HRID 1878521노트

반응식

HRID 1878521 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[N:5]2[N:14]=[C:15]([C:17]3[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=3)[CH:16]=[C:4]2[N:3]=1.[Br:24]N1C(=O)CCC1=O>C(Cl)Cl.[Cl-].[NH4+]>[Br:24][C:16]1[C:15]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)=[N:14][N:5]2[C:6]([N:8]3[CH2:13][CH2:12][O:11][CH2:10][CH2:9]3)=[CH:7][C:2]([Cl:1])=[N:3][C:4]=12

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 58531082HCID 58531082, 화합물

생성물 1

HCID 58531057HCID 58531057, 화합물수율 50.1%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 25517Ammonium Chloride용매

실험 절차

There was dissolved, in methylene chloride (2 mL), 5-chloro-2-(4-methyl-phenyl)-7-morpholin-4-yl-pyrazolo[1,5-a]pyrimidine (44.4 mg, 0.135 mM), then N-bromo-succinimide (27.1 mg, 0.152 mM) was added to the resulting solution and the mixture was stirred at room temperature for 40 minutes. This reaction liquid was diluted with a saturated aqueous ammonium chloride solution and then extracted with methylene chloride. The extracts thus obtained were combined, dried over anhydrous sodium sulfate, the solvent was then distilled off and the resulting residue was purified by the silica gel column chromatography (ethyl acetate/hexane=1:10) to thus obtain the title compound (27.6 mg, yield: 50%).

후처리

  1. customThis reaction liquid
  2. extractionextracted with methylene chloride
  3. customThe extracts thus obtained
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was then distilled off
  6. customthe resulting residue was purified by the silica gel column chromatography (ethyl acetate/hexane=1:10)

출처 및 근거

ORD 기록
ord-25952299163d44e69303bc68d58f064c
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08314098B2

반응 노트

불러오는 중…