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Potassium Carbonate → HCID 54381806, 화합물

HRID 235561
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HRID 235561 반응식
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([O:12][C:13]1[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=1)[CH:6]=[N:5]2.[C:20]([N:22]([CH2:28][CH3:29])[C:23](=[O:27])[CH:24](Br)[CH3:25])#[N:21].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:20]([N:22]([CH2:28][CH3:29])[C:23](=[O:27])[CH:24]([O:19][C:16]1[CH:17]=[CH:18][C:13]([O:12][C:7]2[CH:6]=[N:5][C:4]3[C:9](=[CH:10][CH:11]=[C:2]([F:1])[CH:3]=3)[N:8]=2)=[CH:14][CH:15]=1)[CH3:25])#[N:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 133285004-[(6-Fluoro-2-quinoxalinyl)oxy]phenolHCID 53784648HCID 53784648, 화합물

생성물 1

HCID 54381806HCID 54381806, 화합물수율 48%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

10 g (0.039 mole) of 4-(6-fluoroquinoxalin-2-yloxy)phenol, 9.6 g (0.047 mole) of 2-bromopropionic acid N-cyano-N-ethylamide and 8.1 g (0.058 mole) of potassium carbonate are stirred for 14 hours at room temperature in 100 ml of acetonitrile. The precipitated salts are removed by filtration and the filtrate is concentrated by evaporation. The residue is chromatographed through silica gel eluted with ethyl acetate/hexane (1:3), affording 7.1 g (48% of theory) of 2-[4-(6-fluoroquinoxalin-2-yloxy)phenoxy]propionic acid N-cyano-N-ethylamide with a melting point of 108°-111° C.

후처리

  1. customThe precipitated salts are removed by filtration
  2. concentrationthe filtrate is concentrated by evaporation
  3. customThe residue is chromatographed through silica gel
  4. washeluted with ethyl acetate/hexane (1:3)

출처 및 근거

ORD 기록
ord-edf3c8ef417f4706b64022ee26e87aa1
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04640703

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