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Potassium Carbonate → 2-[4-(6-Chloronicotinoyl]benzylthio]-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

HRID 1291389
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HRID 1291389 반응식
[SH:1][C:2]1[N:3]=[C:4]2[CH:13]=[CH:12][CH:11]=[CH:10][N:5]2[C:6](=[O:9])[C:7]=1[CH3:8].[Cl:14][C:15]1[CH:30]=[CH:29][C:18]([C:19]([C:21]2[CH:28]=[CH:27][C:24]([CH2:25]Br)=[CH:23][CH:22]=2)=[O:20])=[CH:17][N:16]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:14][C:15]1[CH:30]=[CH:29][C:18]([C:19]([C:21]2[CH:28]=[CH:27][C:24]([CH2:25][S:1][C:2]3[N:3]=[C:4]4[CH:13]=[CH:12][CH:11]=[CH:10][N:5]4[C:6](=[O:9])[C:7]=3[CH3:8])=[CH:23][CH:22]=2)=[O:20])=[CH:17][N:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 189188004-(6-Chloronicotinoyl)benzyl bromideHCID 189188982-mercapto-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

생성물 1

HCID 189190212-[4-(6-Chloronicotinoyl]benzylthio]-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one수율 27.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 2-mercapto-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (599 mg), 4-(6-chloronicotinoyl)benzyl bromide (1.179 g) and potassium carbonate (1.148 g) in DMF (40 ml) was stirred at room temperature for 2 hours. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate, washed with water, dried, and concentrated. The residue was recrystallized from tetrahydrofuranethyl acetate to provide the title compound as colorless solid (367 mg).

후처리

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was recrystallized from tetrahydrofuranethyl acetate

출처 및 근거

ORD 기록
ord-1669beb0124e47aa9e44218fbdbd47f5
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753664

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