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Dimethylformamide → HCID 67365819、化合物

HRID 245772
ノート
印刷プレビュー

反応式

HRID 245772 の反応式
[CH3:1][N:2]1[CH2:6][CH:5]([C:7]2[N:11]3[CH:12]=[CH:13][N:14]=[C:15]([CH3:16])[C:10]3=[CH:9][N:8]=2)[CH2:4][C:3]1=[O:17].CN(C)C=O.[Br:23]N1C(=O)CCC1=O>O>[Br:23][C:9]1[N:8]=[C:7]([CH:5]2[CH2:6][N:2]([CH3:1])[C:3](=[O:17])[CH2:4]2)[N:11]2[CH:12]=[CH:13][N:14]=[C:15]([CH3:16])[C:10]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 67184N-bromobutanimideHCID 67363450HCID 67363450、化合物

生成物 1

HCID 67365819HCID 67365819、化合物収率 50.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1-Methyl-4-(8-methylimidazo[1,5-a]pyrazin-3-yl)pyrrolidin-2-one (293 mg, 1.27 mmol) was dissolved N,N-dimethylformamide (12 ml) and N-bromosuccinimide (227 mg, 1.27 mmol) was added and reation mixture was stirred at room temperature overnight. Then water was added to the reaction mixture and extracted with chloroform/iso-propanol (9/1) three times. The combined organic layers were dried (Na2SO4) and concentrated in vacuo and a brown oil was obtained. The residue was purified by column chromatography (silica gel; dichloromethane/methanol/heptane=9/1/4) to give 4-(1-bromo-8-methylimidazo[1,5-a]pyrazin-3-yl)-1-methylpyrrolidin-2-one (200 mg).

後処理

  1. additionwas added
  2. extractionextracted with chloroform/iso-propanol (9/1) three times
  3. dry with materialThe combined organic layers were dried (Na2SO4)
  4. concentrationconcentrated in vacuo
  5. customa brown oil was obtained
  6. customThe residue was purified by column chromatography (silica gel; dichloromethane/methanol/heptane=9/1/4)

出典と根拠

ORDレコード
ord-83770696072244af8e209d0a276ce822
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658794B2

反応ノート

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