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Dimethylformamide → HCID 67365819, 화합물

HRID 245772
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반응식

HRID 245772 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 67184N-bromobutanimideHCID 67363450HCID 67363450, 화합물

생성물 1

HCID 67365819HCID 67365819, 화합물수율 50.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-83770696072244af8e209d0a276ce822
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658794B2

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