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Dimethylformamide → HCID 69204373, 화합물

HRID 2378327
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HRID 2378327 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[C:6](/[CH:12]=[CH:13]/[C:14]#[N:15])[CH:7]=[CH:8][C:9]=1[O:10][CH3:11])[CH3:2].I[C:17]1[CH:18]=[CH:19][C:20]([O:24][CH3:25])=[C:21]([NH2:23])[CH:22]=1.C[C:27]([O-:29])=[O:28].[K+].[CH3:31]N(C=O)C>[N+](CCCC)(CCCC)(CCCC)CCCC.[Br-].CC([O-])=O.CC([O-])=O.[Pd+2]>[CH3:31][O:29][C:27](=[O:28])[NH:23][C:21]1[CH:22]=[CH:17][C:18]([C:12]([C:6]2[CH:7]=[CH:8][C:9]([O:10][CH3:11])=[C:4]([O:3][CH2:1][CH3:2])[CH:5]=2)=[CH:13][C:14]#[N:15])=[CH:19][C:20]=1[O:24][CH3:25].[NH2:23][C:21]1[CH:22]=[CH:17][C:18]([C:12]([C:6]2[CH:7]=[CH:8][C:9]([O:10][CH3:11])=[C:4]([O:3][CH2:1][CH3:2])[CH:5]=2)=[CH:13][C:14]#[N:15])=[CH:19][C:20]=1[O:24][CH3:25]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6228DimethylformamideHCID 517044Potassium AcetateHCID 129053825-Iodo-2-methoxyanilineHCID 53623237HCID 53623237, 화합물

생성물 2

HCID 69204373HCID 69204373, 화합물HCID 77620386HCID 77620386, 화합물

시약·촉매·용매 2

HCID 74236
Tetrabutylammonium Bromide
촉매
HCID 167845palladium(II) acetate촉매

반응 조건

온도
165 °C

실험 절차

In a 20-mL capacity microwave vessel was combined (E)-3-(3-ethoxy-4-methoxyphenyl)-acrylonitrile (0.41 g, 2.0 mmol), 5-iodo-2-methoxy-phenylamine (0.75 g, 1.5 equiv, 3.0 mmol), Pd(OAc)2 (45 mg, 10 mol %, 0.2 mmol), nBu4NBr (0.71 g, 1.1 equiv, 2.2 mmol), and KOAc (0.49 g, 2.5 equiv, 5.0 mmol) in DMF (8 mL). The mixture was purged with nitrogen gas for 30 seconds and the vessel was sealed. The reaction mixture was stirred in a microwave at 165° C. for 50 min, after which the starting material was consumed (TLC). The mixture was diluted with EtOAc (100 mL), washed with water (2×75 mL), and then brine (50 mL). The organic layer was dried (Na2SO4), filtered, and concentrated. The crude material was purified by column chromatography (SiO2, 7:3 hexanes/EtOAc). Concentration of the desired fractions afforded the title compound (Z)-(3-(4-amino-3-methoxy-phenyl)-3-(3-ethoxy-4-methoxy-phenyl)-acrylonitrile in 90% yield, as the major isomer of a 92:8 mixture: 1H NMR δ (400 M Hz, CDCl3) 7.02 (dd, 1H, J=8.4, 2.4 Hz), 6.98 (d, 1H, J=2.4 Hz), 6.90 (d, 1H, J=8.4 Hz), 6.75 (d, 1H, J=8.4 Hz), 6.70 (dd, 1H, J=8.4, 2.4 Hz), 6.65 (d, 1H, J=2.0 Hz), 5.51 (s, 1H), 4.08 (q, 2H, J=6.8 Hz), 3.92 (s, 3H), 3.89 (s, 3H), 1.45 (t, 3H, J=6.8 Hz).

후처리

  1. customIn a 20-mL capacity microwave vessel was combined
  2. customThe mixture was purged with nitrogen gas for 30 seconds
  3. customthe vessel was sealed
  4. customafter which the starting material was consumed (TLC)
  5. additionThe mixture was diluted with EtOAc (100 mL)
  6. washwashed with water (2×75 mL)
  7. dry with materialThe organic layer was dried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe crude material was purified by column chromatography (SiO2, 7:3 hexanes/EtOAc)

출처 및 근거

ORD 기록
ord-d4c61104eba445bd8fbfda65eee28424
출처 데이터셋
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07470723B2

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