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Cesium fluoride → 8-(3,5-Dimethylisoxazol-4-yl)-6-fluoro-3-pyridin-3-yl-2H-1,4-benzoxazin-5-amine

HRID 928555
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HRID 928555 반응식
[F-].[Cs+].Br[C:4]1[CH:5]=[C:6]([F:21])[C:7]([NH2:20])=[C:8]2[C:13]=1[O:12][CH2:11][C:10]([C:14]1[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=1)=[N:9]2.[CH3:22][C:23]1[C:27](B(O)O)=[C:26]([CH3:31])[O:25][N:24]=1>C(O)CCC.O.C(P(C(C)(C)C)C1C=CC(N(C)C)=CC=1)(C)(C)C.Cl[Pd]Cl>[CH3:22][C:23]1[C:27]([C:4]2[CH:5]=[C:6]([F:21])[C:7]([NH2:20])=[C:8]3[C:13]=2[O:12][CH2:11][C:10]([C:14]2[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=2)=[N:9]3)=[C:26]([CH3:31])[O:25][N:24]=1
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참가 물질

7

반응물 3

HCID 25953Cesium fluorideHCID 27343463,5-Dimethylisoxazole-4-boronic acidHCID 904091678-Bromo-6-fluoro-3-pyridin-3-yl-2H-1,4-benzoxazin-5-amine

생성물 1

HCID 1177775028-(3,5-Dimethylisoxazol-4-yl)-6-fluoro-3-pyridin-3-yl-2H-1,4-benzoxazin-5-amine수율 80%

시약·촉매·용매 3

HCID 86647055
di-tert-butyl(4-dimethylaminophenylphosphine) dichloropalladium(II)
촉매
HCID 2631-Butanol용매
HCID 962Water용매

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온도
100 °C

실험 절차

4-(Di-tert-butylphosphino)-N,N-dimethylaniline-dichloropalladium (2:1) (3.3 mg, 0.0047 mmol) and cesium fluoride (83 mg, 0.54 mmol), 8-bromo-6-fluoro-3-pyridin-3-yl-2H-1,4-benzoxazin-5-amine (50 mg, 0.2 mmol) and (3,5-dimethylisoxazol-4-yl)boronic acid (33 mg, 0.23 mmol) were stirred in 1-butanol (0.50 mL) and water (0.12 mL). The system was placed under vacuum and back-filled with nitrogen (repeated 3×) while stirring the suspension. The mixture was further degassed by bubbling nitrogen through the solution for 10 minutes. The mixture was heated at 100° C. for 1 hour. Extractive workup with ethyl acetate gave the desired compound 40 mg, 80%. 1H NMR (300 MHz, DMSO-d6) δ 9.28 (s, 1H), 8.68 (m, 1H), 8.51 (m, 1H), 7.52 (m, 1H), 6.89 (m, 1H), 5.80 (s, 2H), 5.13 (s, 2H), 2.25 (s, 3H), 2.10 (s, 3H). LCMS calculated for C18H16FN4O2 (M+H)+: m/z=339.1. found: 339.0.

후처리

  1. additionback-filled with nitrogen (repeated 3×)
  2. customThe mixture was further degassed
  3. customby bubbling nitrogen through the solution for 10 minutes

출처 및 근거

ORD 기록
ord-1086bf9bee0048a6aca8ee1563d6fe34
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09290514B2

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