N-bromobutanimide → HCID 58531057、化合物

HRID 1878521ノート

反応式

HRID 1878521 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]=[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

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 58531082HCID 58531082、化合物

生成物 1

HCID 58531057HCID 58531057、化合物収率 50.1%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 25517Ammonium Chloride溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-25952299163d44e69303bc68d58f064c
出典データセット
uspto-grants-2012_11
特許番号
US08314098B2

反応ノート

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