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Potassium Carbonate → 6-Acetoxy-5-oxo-1-(2-oxo-2-piperidin-1-yl-ethyl)-1,5-dihydro-imidazo[1,2-a]pyrimidine-7-carboxylic acid methyl ester

HRID 1971814
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HRID 1971814 반응식
[CH3:1][O:2][C:3]([C:5]1[N:6]=[C:7]2[NH:18][CH:17]=[CH:16][N:8]2[C:9](=[O:15])[C:10]=1[O:11][C:12](=[O:14])[CH3:13])=[O:4].Cl[CH2:20][C:21]([N:23]1[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]1)=[O:22].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[CH3:1][O:2][C:3]([C:5]1[N:6]=[C:7]2[N:18]([CH2:20][C:21](=[O:22])[N:23]3[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]3)[CH:17]=[CH:16][N:8]2[C:9](=[O:15])[C:10]=1[O:11][C:12](=[O:14])[CH3:13])=[O:4]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2223122-Chloro-1-piperidine-1-yl-ethanoneHCID 178499055HCID 178499055, 화합물

생성물 1

HCID 581269386-Acetoxy-5-oxo-1-(2-oxo-2-piperidin-1-yl-ethyl)-1,5-dihydro-imidazo[1,2-a]pyrimidine-7-carboxylic acid methyl ester수율 66.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of compound 6-acetoxy-5-oxo-1,5-dihydro-imidazo[1,2-a]pyrimidine-7-carboxylic acid methyl ester (PCT/AU2007/001980) (2.0 g, 7.96 mmol) in anhydrous acetonitrile (20 ml) was added compound 2-chloro-1-piperidin-1-yl-ethanone (2.0 g, 12.42 mmol), K2CO3 (1.7 g, 12.32 mmol), KI (133 mg, 0.8 mmol) successively. The mixture was heated at refluxed for 3 hours. After cooling to the room temperature, the mixture was filtered and the filtrate was concentrated under reduced pressure. The resulting residue was recrystallized from ethyl acetate to give titled compound (2.0 g, yield 66.7%).

후처리

  1. temperatureThe mixture was heated
  2. temperatureat refluxed for 3 hours
  3. filtrationthe mixture was filtered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe resulting residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-585e35198dad4498bd92c9826ca2fca8
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08431581B2

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