Water → HCID 2915197, 화합물

HRID 1282084노트

반응식

HRID 1282084 반응식
[C:1]([N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1)(=[O:3])[CH3:2].F[C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=1[N+:18]([O-:20])=[O:19].C(=O)([O-])[O-].[K+].[K+].O>C(#N)C>[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=2[N+:18]([O-:20])=[O:19])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 677672,5-DifluoronitrobenzeneHCID 837951-Acetylpiperazine

생성물 1

HCID 2915197HCID 2915197, 화합물수율 86.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 1-acetylpiperazine (20 g) in acetonitrile (50 ml) were added 2,5-difluoronitrobenzene (25 g) and potassium carbonate (22 g) and the mixture was refluxed under heating at room temperature for 4.5 hr. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated to give a red oil. The oil was crystallized from ethyl acetate-isopropyl ether to give the title compound (36 g) as a red solid.

후처리

  1. temperaturethe mixture was refluxed
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated
  6. customto give a red oil
  7. customThe oil was crystallized from ethyl acetate-isopropyl ether

출처 및 근거

ORD 기록
ord-9f3b9fcbb6d2486d92c6716417e52ca1
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06455528B1

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