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2-(Methylsulfonyl)phenylboronic Acid → 5-(3-Fluoro-2'-(methylsulfonyl)-[1,1'-biphenyl]-4-yl)pyrazin-2-amine

HRID 1523773
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HRID 1523773 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[CH:10][C:11]([NH2:14])=[N:12][CH:13]=2)=[C:4]([F:15])[CH:3]=1.[CH3:16][S:17]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1B(O)O)(=[O:19])=[O:18]>CC(C1C=C(C(C)C)C(C2C=CC=C(P(C3CCCCC3)C3CCCCC3)C=2)=C(C(C)C)C=1)C.C1C=[C-]C(C2C(N)=CC=CC=2)=CC=1.Cl[Pd+]>[F:15][C:4]1[CH:3]=[C:2]([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[S:17]([CH3:16])(=[O:19])=[O:18])[CH:7]=[CH:6][C:5]=1[C:8]1[N:9]=[CH:10][C:11]([NH2:14])=[N:12][CH:13]=1
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참가 물질

4

반응물 2

HCID 27735392-(Methylsulfonyl)phenylboronic AcidHCID 802004855-(4-Chloro-2-fluorophenyl)pyrazin-2-amine

생성물 1

HCID 778446965-(3-Fluoro-2'-(methylsulfonyl)-[1,1'-biphenyl]-4-yl)pyrazin-2-amine수율 90.2%

시약·촉매·용매 1

HCID 72376365[2-(2-Aminophenyl)phenyl]-chloro-palladium dicyclohexyl-[3-(2,4,6-triisopropylphenyl)phenyl]phosphane촉매

실험 절차

To a nitrogen sparged flask containing 5-(4-chloro-2-fluorophenyl)pyrazin-2-amine (34.0 g, 152 mmol), 2-methylsulfonylphenylboronic acid (38.0 g, 190 mmol), and chloro(2-dicyclohexylphosphino-2′,4′,6′-triisopropyl-1,1′-biphenyl)[2-(2′-amino-1,1′-biphenyl)]palladium(II) (2.39 g, 3.0 mmol) were added sparged THF (300 mL) and K3PO4(aq) (608 mL, 0.5 M). The mixture was stirred for 15 hours at rt and then concentrated under reduced pressure to remove the THF. The remaining portion was treated with toluene (325 mL) and THF (25 mL). The biphasic slurry was stirred for 20 h at rt and then filtered and the isolated solid washed with water (150 mL) and toluene (150 mL). The filter cake was dried to provide the title compound (47.1 g, 90%). MS (ESI): mass calcd. for C17H14FN3O2S, 343.08; m/z found, 344.1 [M+H]+. 1H NMR (400 MHz, DMSO-d6) δ 8.41 (dd, J=2.4, 1.5, 1H), 8.12 (dd, J=7.9, 1.4, 1H), 8.04 (d, J=1.5, 1H), 7.93 (m, 1H), 7.80 (m, 1H), 7.72 (m, 1H), 7.48 (dd, J=7.6, 1.4, 1H), 7.37 (dd, J=12.3, 1.7, 1H), 7.32 (dd, J=8.1, 1.7, 1H), 6.76 (s, 2H), 2.95 (s, 3H).

후처리

  1. additionwere added
  2. customsparged THF (300 mL) and K3PO4(aq) (608 mL, 0.5 M)
  3. concentrationconcentrated under reduced pressure
  4. customto remove the THF
  5. additionThe remaining portion was treated with toluene (325 mL) and THF (25 mL)
  6. stirringThe biphasic slurry was stirred for 20 h at rt
  7. filtrationfiltered
  8. washthe isolated solid washed with water (150 mL) and toluene (150 mL)
  9. customThe filter cake was dried

출처 및 근거

ORD 기록
ord-e0149b7ab9984c94a14fd0666a62473b
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09079866B2

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