N-bromobutanimide → 3-Bromo-5-chloro-7-morpholin-4-yl-pyrazolo[1,5-a]pyrimidine

HRID 1878528노트

반응식

HRID 1878528 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]=[CH:15][CH:16]=[C:4]2[N:3]=1.[Br:17]N1C(=O)CCC1=O>C(Cl)Cl.C(=O)(O)[O-].[Na+]>[Br:17][C:16]1[CH:15]=[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 585310715-Chloro-7-morpholin-4-yl-pyrazolo[1,5-a]pyrimidine

생성물 1

HCID 585310033-Bromo-5-chloro-7-morpholin-4-yl-pyrazolo[1,5-a]pyrimidine수율 61%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 516892Sodium Bicarbonate용매

실험 절차

There was dissolved, in methylene chloride (2 mL), 5-chloro-7-morpholin-4-yl-pyrazolo[1,5-a]pyrimidine (100 mg, 0.419 mM), then N-bromo-succinimide (78.8 mg, 0.443 mM) was added to the solution and the mixture was stirred at room temperature for one hour. This reaction liquid was diluted with a saturated aqueous sodium bicarbonate solution and then extracted with ethyl acetate. The extracts thus obtained were combined, dried over anhydrous sodium sulfate and the solvent was then distilled off. The resulting residue was purified by the silica gel column chromatography (methylene chloride) to thus give the title compound (80.7 mg, yield: 61%).

후처리

  1. customThis reaction liquid
  2. extractionextracted with ethyl acetate
  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 (methylene chloride)

출처 및 근거

ORD 기록
ord-2068f934617a4756a3adfe7cbbc13970
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08314098B2

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