Hydrochloric Acid → 2-(4,6-Dimethoxypyrimidine-2-yl)-2-(2-nitrophenyl)acetonitrile

HRID 989600

반응식

HRID 989600 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH2:10][C:11]#[N:12])([O-:3])=[O:2].[H-].[Na+].[CH3:15][O:16][C:17]1[CH:22]=[C:21]([O:23][CH3:24])[N:20]=[C:19](S(C)(=O)=O)[N:18]=1.Cl>CN(C)C=O.O>[CH3:15][O:16][C:17]1[CH:22]=[C:21]([O:23][CH3:24])[N:20]=[C:19]([CH:10]([C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N+:1]([O-:3])=[O:2])[C:11]#[N:12])[N:18]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 118882-NitrophenylacetonitrileHCID 24758Sodium hydrideHCID 8383634,6-Dimethoxy-2-(methylsulfonyl)pyrimidine

생성물 1

HCID 184179902-(4,6-Dimethoxypyrimidine-2-yl)-2-(2-nitrophenyl)acetonitrile수율 79.2%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

50 g (0.31 M) of 2-(2-nitrophenyl)acetonitrile was dissolved in 500 ml of dimethylformamide. Thereto was added 24.7 g (0.62 M) of 60% sodium hydride. The mixture was stirred at room temperature for 2 hours. Then, 68 g (0.31 M) of 4,6-dimethoxy-2-methanesulfonylpyrimidine was added. The mixture was stirred at 80° C. for 1 hour to give rise to a reaction. The reaction mixture was poured into water, followed by neutralization with dilute hydrochloric acid. The mixture was subjected to extraction with ethyl acetate. The extract was washed with water, dried and subjected to vacuum distillation to remove the solvent. The residue was recrystallized from ethanol to obtain 73.3 g (yield: 79%) of 2-(4,6-dimethoxypyrimidine-2-yl)-2-(2-nitrophenyl)acetonitrile as a white powder (melting point: 88 to 89° C.).

후처리

  1. stirringThe mixture was stirred at 80° C. for 1 hour
  2. customto give rise
  3. customto a reaction
  4. extractionThe mixture was subjected to extraction with ethyl acetate
  5. washThe extract was washed with water
  6. customdried
  7. distillationsubjected to vacuum distillation
  8. customto remove the solvent
  9. customThe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-dd022a877f0f4698bbe28d430fdf74a2
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06458748B1

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