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Water → 1-Acetyl-4-(4,6-difluoropyrimidin-2-yl)piperazine

HRID 1282153
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HRID 1282153 반응식
[F:1][C:2]1[N:7]=[C:6]([F:8])[CH:5]=[C:4]([F:9])[N:3]=1.C(=O)([O-])[O-].[K+].[K+].[C:16]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)(=[O:18])[CH3:17].O>C(#N)C>[C:16]([N:19]1[CH2:24][CH2:23][N:22]([C:2]2[N:7]=[C:6]([F:8])[CH:5]=[C:4]([F:9])[N:3]=2)[CH2:21][CH2:20]1)(=[O:18])[CH3:17].[C:16]([N:19]1[CH2:24][CH2:23][N:22]([C:6]2[CH:5]=[C:4]([F:9])[N:3]=[C:2]([F:1])[N:7]=2)[CH2:21][CH2:20]1)(=[O:18])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 696772,4,6-TrifluoropyrimidineHCID 837951-Acetylpiperazine

생성물 2

HCID 184230501-Acetyl-4-(4,6-difluoropyrimidin-2-yl)piperazineHCID 184231521-Acetyl-4-(2,6-difluoropyrimidin-4-yl)piperazine

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

To a solution of 2,4,6-trifluoropyrimidine (2.0 g) and potassium carbonate (3.1 g) in acetonitrile (15 ml) was added a solution of 1-acetylpiperazine (1.9 g) in acetonitrile (5 ml) over 10 min under ice-cooling and the mixture was stirred at room temperature for 1 hr. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with brine and dried over anhydrous sodium sulfate. The solvent was evaporated to give a pale-yellow oil. The obtained pale-yellow oil was purified by silica gel column chromatography to give the title compound (1.8 g) and 1-acetyl-4-(2,6-difluoropyrimidin-4-yl)piperazine (1.7 g) both as a white solid.

후처리

  1. temperaturecooling
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated
  6. customto give a pale-yellow oil
  7. customThe obtained pale-yellow oil was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-b2048bc1cd7a4f399b5faa32651e1386
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06455528B1

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