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Cesium carbonate → Tert-butyl 4-(3-fluoro-4-nitrophenyl)piperazine-1-carboxylate

HRID 1503837
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HRID 1503837 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([F:11])[CH:3]=1.[N:12]1([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+]>C1(C)C=CC=CC=1.C([O-])(=O)C.C([O-])(=O)C.[Pd+2]>[F:11][C:4]1[CH:3]=[C:2]([N:15]2[CH2:14][CH2:13][N:12]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17][CH2:16]2)[CH:7]=[CH:6][C:5]=1[N+:8]([O-:10])=[O:9]
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참가 물질

7

반응물 4

HCID 10796Cesium carbonateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 634876Binap, (A+-)-HCID 27833624-Bromo-2-fluoro-1-nitrobenzene

생성물 1

HCID 66738172Tert-butyl 4-(3-fluoro-4-nitrophenyl)piperazine-1-carboxylate

시약·촉매·용매 2

HCID 167845
palladium(II) acetate
촉매
HCID 1140Toluene용매

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온도
60 °C

실험 절차

A mixture of 4-bromo-2-fluoro-1-nitrobenzene (5 g, 23 mmol), tert-butyl piperazine-1-carboxylate (4.24 g, 23 mmol), palladium diacetate (0.51 g, 2.3 mmol), (±)-2,2′-bis(diphenylphosphino)-1,1′-binaphthalene (2.13 g, 3.4 mmol) and cesium carbonate (14.8 g, 45 mmol) in toluene (120 mL) was heated under nitrogen at 60° C. for 20 hours. After cooling to ambient temperature, the mixture was concentrated and the residue was diluted with dichloromethane (300 mL) and washed with water. The combined organic phase was washed with brine, dried over sodium sulfate, filtered and concentrated. The residue was purified by flash chromatography on silica gel (200-300 mesh) eluting with 3/1 petroleum ether/ethyl acetate to give the title compound. MS: 348 (M+Na+).

후처리

  1. temperatureAfter cooling to ambient temperature
  2. concentrationthe mixture was concentrated
  3. additionthe residue was diluted with dichloromethane (300 mL)
  4. washwashed with water
  5. washThe combined organic phase was washed with brine
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was purified by flash chromatography on silica gel (200-300 mesh)
  10. washeluting with 3/1 petroleum ether/ethyl acetate

출처 및 근거

ORD 기록
ord-00247088b5204658aeb726e825d46038
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09212192B2

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