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Methanol → HCID 178493783, 화합물

HRID 525277
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HRID 525277 반응식
Br[C:2]1[CH:3]=[N:4][C:5]([NH:8][C@H:9]2[CH2:14][CH2:13][C@@H:12]([O:15][C:16]3[CH:25]=[C:24]([N:26]4[CH2:31][CH2:30][O:29][CH2:28][CH2:27]4)[CH:23]=[C:22]4[C:17]=3[N:18]=[CH:19][CH:20]=[N:21]4)[CH2:11][CH2:10]2)=[N:6][CH:7]=1.[C:32](=O)([O-])[O-:33].[Cs+].[Cs+].CO>C1(C)C=CC=CC=1.[CH2-]C=C.[CH2-]C=C.Cl[Pd+].Cl[Pd+].CC1C=CC(OC)=C(P(C(C)(C)C)C(C)(C)C)C=1C1C(C(C)C)=CC(C(C)C)=CC=1C(C)C>[CH3:32][O:33][C:2]1[CH:3]=[N:4][C:5]([NH:8][C@H:9]2[CH2:14][CH2:13][C@@H:12]([O:15][C:16]3[CH:25]=[C:24]([N:26]4[CH2:31][CH2:30][O:29][CH2:28][CH2:27]4)[CH:23]=[C:22]4[C:17]=3[N:18]=[CH:19][CH:20]=[N:21]4)[CH2:11][CH2:10]2)=[N:6][CH:7]=1
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참가 물질

7

반응물 3

HCID 887MethanolHCID 10796Cesium carbonateHCID 178419459HCID 178419459, 화합물

생성물 1

HCID 178493783HCID 178493783, 화합물수율 63.6%

시약·촉매·용매 3

HCID 61538Palladium, di-mu-chlorobis(eta3-2-propenyl)di-촉매
HCID 56641709
(2',4'-Diisopropyl-3-methoxy-6-methyl-6'-propyl-2-biphenylyl)[bis(2-methyl-2-propanyl)]phosphine
촉매
HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

As shown in step 6-ix of Scheme 6, to a mixture 5-bromo-N-((cis)-4-((7-morpholinoquinoxalin-5-yl)oxy)cyclohexyl)pyrimidin-2-amine (75 mg, 0.155 mmol), cesium carbonate (101 mg, 0.309 mmol), allylpalladium(II) chloride dimer (0.28 mg, 0.0015 mmol), RockPhos (2.17 mg, 0.0046 mmol) and MeOH (9.9 mg, 12.5 μL, 0.31 mmol) in toluene (2 mL) was flushed with nitrogen gas and heated to 100° C. for 18 hours. The reaction mixture was iluted with EtOAc, filtered though a layer of diatomaceous earth, and concentrated under reduced pressure. Purification by medium pressure silica gel chromatography (0-8% MeOH/DCM gradient) yielded 5-methoxy-N-((cis)-4-((7-morpholinoquinoxalin-5-yl)oxy)cyclohexyl)pyrimidin-2-amine (compound 134, 43 mg): 1H-NMR (300 MHz, CDCl3) δ 8.70 (d, J=1.9 Hz, 1H), 8.63 (d, J=1.9 Hz, 1H), 8.07 (s, 2H), 6.96 (d, J=2.5 Hz, 1H), 6.92 (d, J=2.5 Hz, 1H), 5.01 (d, J=8.1 Hz, 1H), 4.80 (q, J=5.6, 4.2 Hz, 1H), 4.03-3.87 (m, 5H), 3.80 (s, 3H), 3.42-3.27 (m, 4H), 2.29-2.10 (m, 2H), 1.99-1.82 (m, 6H).

후처리

  1. customwas flushed with nitrogen gas
  2. filtrationfiltered though a layer of diatomaceous earth
  3. concentrationconcentrated under reduced pressure
  4. customPurification by medium pressure silica gel chromatography (0-8% MeOH/DCM gradient)

출처 및 근거

ORD 기록
ord-d6003b3d339d450aa097cff3708b1d00
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09340557B2

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