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

HRID 1878528ノート

反応式

HRID 1878528 の反応式
[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

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 585310715-Chloro-7-morpholin-4-yl-pyrazolo[1,5-a]pyrimidine

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-2068f934617a4756a3adfe7cbbc13970
出典データセット
uspto-grants-2012_11
特許番号
US08314098B2

反応ノート

読み込み中…