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Cesium fluoride → HCID 89924280, 화합물

HRID 1505698
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HRID 1505698 반응식
N[C:2]1[CH:3]=[C:4]([C:8]2[N:13]=[CH:12][C:11]([C:14]3[CH:15]=[N:16][N:17]([CH:19]4[CH2:24][CH2:23][N:22]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:21][CH2:20]4)[CH:18]=3)=[CH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.[O:32]1[CH:36]=[C:35](B2OC(C)(C)C(C)(C)O2)[CH:34]=[N:33]1.[F-].[Cs+].O1CCOCC1>CCOC(C)=O.O.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl>[O:32]1[CH:36]=[C:35]([C:2]2[CH:3]=[C:4]([C:8]3[N:13]=[CH:12][C:11]([C:14]4[CH:15]=[N:16][N:17]([CH:19]5[CH2:20][CH2:21][N:22]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:23][CH2:24]5)[CH:18]=4)=[CH:10][N:9]=3)[CH:5]=[CH:6][CH:7]=2)[CH:34]=[N:33]1
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참가 물질

8

반응물 4

HCID 25953Cesium fluorideHCID 312751,4-DioxaneHCID 164141804-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2-oxazoleHCID 89924531HCID 89924531, 화합물2회

생성물 1

HCID 89924280HCID 89924280, 화합물수율 62%

시약·촉매·용매 3

HCID 6102075
Dichlorobis(triphenylphosphine)palladium
촉매
HCID 962Water용매2회
HCID 8857Ethyl Acetate용매

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온도
120 °C

실험 절차

Tert-butyl 4-4-[2-(3-iodophenyl)pyrimidin-5-yl]-1H-pyrazol-1-ylpiperidine-1-carboxylate (intermediate 5, 150 mg; 0.24 mmol; 1.0 eq.), 4-Isoxazoleboronic acid pinacol ester (47 mg; 0.24 mmol; 1.0 eq.), bis(triphenylphosphine)palladium(II)chloride (17 mg; 0.02 mmol; 0.10 eq.) and cesium fluoride (109 mg; 0.72 mmol; 3.0 eq.) were flushed with nitrogen before the addition of dioxane: water (2.25:1.1 mL). The reaction mixture was heated in MW at 120° C. for 30 min. It was then diluted with EtOAc and water. Aqueous phase was extracted with EtOAc and combined organic phases were dried over magnesium sulfate, filtered and concentrated. Purification by flash chromatography (cyclohexane:EtOAc, gradient from 80:20 to 30:70) afforded the title compound as a white beige solid (70 mg; 62%). 1H NMR (300 MHz, DMSO-d6) δ 9.60 (s, 1H), 9.27 (s, 1H), 9.17 (s, 2H), 8.64 (t, J=1.5 Hz, 1H), 8.56 (s, 1H), 8.35 (dt, J=8.0 Hz, 1.5 Hz, 1H), 8.16 (s, 1H), 7.87-7.83 (m, 1H), 7.61 (t, J=8.0 Hz, 1H), 4.47-4.35 (m, 1H), 4.09-4.04 (m, 2H), 2.95 (m, 2H), 2.09-2.06 (m, 2H), 1.87-1.72 (m, 2H), 1.43 (s, 9H). HPLC (Condition A): Rt 4.70 min (purity 97.4%). MS (ESI+): 473.5.

후처리

  1. extractionAqueous phase was extracted with EtOAc
  2. dry with materialwere dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customPurification by flash chromatography (cyclohexane:EtOAc, gradient from 80:20 to 30:70)

출처 및 근거

ORD 기록
ord-92ec2279202740a6803f63f1602b1fbb
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216991B2

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