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Water → N-(4-((4-(4,6-dimethoxypyrimidin-2-yl)piperazin-1-yl)methyl)phenylmethyl)acetamide

HRID 1282154
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HRID 1282154 반응식
Cl[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][NH:10][C:11](=[O:13])[CH3:12])=[CH:5][CH:4]=1.[CH3:14][O:15][C:16]1[CH:21]=[C:20]([O:22][CH3:23])[N:19]=[C:18]([N:24]2[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]2)[N:17]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:14][O:15][C:16]1[CH:21]=[C:20]([O:22][CH3:23])[N:19]=[C:18]([N:24]2[CH2:25][CH2:26][N:27]([CH2:2][C:3]3[CH:8]=[CH:7][C:6]([CH2:9][NH:10][C:11](=[O:13])[CH3:12])=[CH:5][CH:4]=3)[CH2:28][CH2:29]2)[N:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 50909284,6-Dimethoxy-2-(piperazin-1-yl)pyrimidineHCID 15550682N-((4-(chloromethyl)phenyl)methyl)acetamide

생성물 1

HCID 11574555N-(4-((4-(4,6-dimethoxypyrimidin-2-yl)piperazin-1-yl)methyl)phenylmethyl)acetamide수율 123.8%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

A solution of N-(4-chloromethylphenylmethyl) acetamide (0.93 g), 1-(4,6-dimethoxypyrimidin-2-yl)piperazine (0.94 g) and potassium carbonate (0.97 g) in dimethylformamide (10 ml) was stirred at 80° C. for 1.5 hr. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated to give a brown oil (2.0 g). The obtained brown oil was crystallized from ethyl acetate:diisopropyl ether(1:3, 40 ml) to give the title compound (1.3 g) as pale-yellow crystals, m.p.=130-131° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-2807e4f683aa435da3759e1bdb15c791
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06455528B1

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