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Pyridine → 7-bromo-5-fluoro-1-{3-fluoro-4-[(phenylmethyl)oxy]phenyl}-4-[(phenylmethyl)oxy]-1H-indole

HRID 2421230
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HRID 2421230 반응식
[Br:1][C:2]1[CH:3]=[C:4]([F:19])[C:5]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:6]2[C:10]=1[NH:9][CH:8]=[CH:7]2.[F:20][C:21]1[CH:22]=[C:23](B(O)O)[CH:24]=[CH:25][C:26]=1[O:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.N1C=CC=CC=1.B(O)O>ClCCl.C(OCC)(=O)C.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[Br:1][C:2]1[CH:3]=[C:4]([F:19])[C:5]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:6]2[C:10]=1[N:9]([C:23]1[CH:24]=[CH:25][C:26]([O:27][CH2:28][C:29]3[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=3)=[C:21]([F:20])[CH:22]=1)[CH:8]=[CH:7]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 1049Pyridine2회HCID 61668Boronic Acid2회HCID 27377884-Benzyloxy-3-fluorophenylboronic AcidHCID 583038564-(benzyloxy)-7-bromo-5-fluoro-1H-indole

생성물 1

HCID 596279357-bromo-5-fluoro-1-{3-fluoro-4-[(phenylmethyl)oxy]phenyl}-4-[(phenylmethyl)oxy]-1H-indole수율 30%

시약·촉매·용매 3

HCID 8895Cupric acetate촉매2회
HCID 6344Dichloromethane용매
HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 7-bromo-5-fluoro-4-[(phenylmethyl)oxy]-1H-indole (D5) (3 g, 9.37 mmol), {3-fluoro-4-[(phenylmethyl)oxy]phenyl}boronic acid (3.46 g, 14.06 mmol), copper (II) acetate (2.55 g, 14.06 mmol) and pyridine (0.834 mL, 0.815 g, 10.31 mmol) in dichloromethane (50 mL) were stirred together vigorously under an air atmosphere with powdered 4A molecular sieves (˜10 g). After stirring for 20 hours, another 0.5 g of boronic acid were added and the mixture was stirred for a further 24 hours. Then another 1.73 g boronic acid (0.75 eq), copper acetate (1.28 g, 0.75 eq) and pyridine (1.52 mL, 2 eq) were added and stirring was continued at room temperature. After a further 24 hours, the reaction was diluted with ethyl acetate and filtered through celite. The celite was washed with ethyl acetate and the combined filtrates were washed with water (2×), dried (Na2SO4) and concentrated. Chromatography SP4 (0-30% ethyl acetate in hexane) gave the title compound as a white solid (D6), (1.463 g).

후처리

  1. stirringthe mixture was stirred for a further 24 hours
  2. stirringstirring
  3. customwas continued at room temperature
  4. waitAfter a further 24 hours
  5. filtrationfiltered through celite
  6. washThe celite was washed with ethyl acetate
  7. washthe combined filtrates were washed with water (2×)
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-09c761198be24bf9a6dd5fea6443048a
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07956083B2

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