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Acetonitrile → Methyl 4-amino-5-fluoro-6-(4-formylphenyl)-3-vinylpicolinate

HRID 516561
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HRID 516561 반응식
[F-].[K+].[NH2:3][C:4]1[C:9]([F:10])=[C:8](Cl)[N:7]=[C:6]([C:12]([O:14][CH3:15])=[O:13])[C:5]=1[CH:16]=[CH2:17].CC1(C)C(C)(C)OB([C:26]2[CH:33]=[CH:32][C:29]([CH:30]=[O:31])=[CH:28][CH:27]=2)O1.C(#N)C>C(Cl)Cl.O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[NH2:3][C:4]1[C:9]([F:10])=[C:8]([C:26]2[CH:33]=[CH:32][C:29]([CH:30]=[O:31])=[CH:28][CH:27]=2)[N:7]=[C:6]([C:12]([O:14][CH3:15])=[O:13])[C:5]=1[CH:16]=[CH2:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6342AcetonitrileHCID 522689Potassium FluorideHCID 27695364-Formylphenylboronic acid pinacol esterHCID 86668309Methyl 4-amino-6-chloro-5-fluoro-3-vinylpicolinate

생성물 1

HCID 90408697Methyl 4-amino-5-fluoro-6-(4-formylphenyl)-3-vinylpicolinate수율 97.5%

시약·촉매·용매 3

HCID 178418476
HCID 178418476, 화합물
촉매
HCID 962Water용매2회
HCID 6344Dichloromethane용매

실험 절차

To a 5-mL microwave safe vial was added potassium fluoride (0.378 g, 6.50 mmol), methyl 4-amino-6-chloro-5-fluoro-3-vinylpicolinate (0.5 g, 2.168 mmol), bis(triphenylphosphine)palladium(II) chloride (0.152 g, 0.217 mmol) and 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzaldehyde (0.528 g, 2.276 mmol). A mixture of water (1 mL) and acetonitrile (2 mL) was added and the reaction was capped and placed in a Biotage Initiator™ microwave reactor for 20 min at 115° C., with external IR-sensor temperature monitoring from the side of the vessel. Upon cooling to room temperature, the reaction mixture was diluted with CH2Cl2 (25 mL) and water (25 mL) and the organic layer was filtered through a cotton plug. An additional extraction using EtOAc (25 mL) was combined with the CH2Cl2 and dried over Na2SO4 (50 g). Following filtration of the combined organics through a cotton plug and concentration on a rotary evaporator, the residue was purified using a Teledyne ISCO purification system with a gradient eluent system of CH2Cl2 and EtOAc to yield the title compound as a white solid (635 mg): 1H NMR (400 MHz, CDCl3) δ 10.08 (s, 1H), 8.13 (dd, J=8.3, 1.6 Hz, 2H), 8.03-7.93 (m, 2H), 6.91 (ddd, J=18.1, 11.6, 0.5 Hz, 1H), 5.73 (dd, J=11.5, 1.4 Hz, 1H), 5.60 (dd, J=18.1, 1.4 Hz, 1H), 4.77 (s, 2H), 3.94 (s, 3H); 19F NMR (376 MHz, CDCl3) δ −143.49; ESIMS m/z 301 ([M+H]+).

후처리

  1. additionwas added
  2. customthe reaction was capped
  3. filtrationthe organic layer was filtered through a cotton plug
  4. extractionAn additional extraction
  5. dry with materialdried over Na2SO4 (50 g)
  6. filtrationfiltration of the
  7. concentrationcombined organics through a cotton plug and concentration
  8. customon a rotary evaporator
  9. customthe residue was purified
  10. customa Teledyne ISCO purification system with a gradient eluent system of CH2Cl2 and EtOAc

출처 및 근거

ORD 기록
ord-d87fce373ac541c1976e08eed4adf297
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09113629B2

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