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Diethyl Malonate → 2-(7-((3,4-Difluorobenzyl)oxy)-1,5-naphthyridin-3-yl)acetamide

HRID 513965
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HRID 513965 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:23]=[CH:24][C:25]=1[F:26])[CH2:5][O:6][C:7]1[CH:16]=[C:15]2[C:10]([CH:11]=[C:12]([CH2:17][C:18](OCC)=[O:19])[CH:13]=[N:14]2)=[N:9][CH:8]=1.BrC1C=[N:30]C2C(C=1)=NC=C(OCC1C=CC(F)=C(F)C=1)C=2.F[B-](F)(F)F.C([PH+](C(C)(C)C)C(C)(C)C)(C)(C)C.P([O-])([O-])([O-])=O.[K+].[K+].[K+].O1CCOCCOCCOCCOCCOCC1.C(OCC)(=O)CC(OCC)=O>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[F:1][C:2]1[CH:3]=[C:4]([CH:23]=[CH:24][C:25]=1[F:26])[CH2:5][O:6][C:7]1[CH:16]=[C:15]2[C:10]([CH:11]=[C:12]([CH2:17][C:18]([NH2:30])=[O:19])[CH:13]=[N:14]2)=[N:9][CH:8]=1
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참가 물질

8

반응물 6

HCID 7761Diethyl MalonateHCID 2855718-Crown-6HCID 62657Potassium Phosphate, TribasicHCID 2734635Tri-tert-butylphosphine tetrafluoroborateHCID 90416945Ethyl 2-(7-((3,4-difluorobenzyl)oxy)-1,5-naphthyridin-3-yl)acetateHCID 904175933-Bromo-7-((3,4-difluorobenzyl)oxy)-1,5-naphthyridine

생성물 1

HCID 862968492-(7-((3,4-Difluorobenzyl)oxy)-1,5-naphthyridin-3-yl)acetamide수율 53.8%

시약·촉매·용매 1

HCID 9811564Bis(dibenzylideneacetone)palladium촉매

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온도
115 °C

실험 절차

Ethyl 2-(7-((3,4-difluorobenzyl)oxy)-1,5-naphthyridin-3-yl)acetate. 3-Bromo-7-((3,4-difluorobenzyl)oxy)-1,5-naphthyridine (3.20 g, 9.11 mmol), Pd2(dba)3 (41.72 mg, 0.05 mmol), tri-tert-butylphosphonium tetrafluoroborate (290.84 mg, 1 mmol), potassium phosphate (5.42 g, 25.52 mmol), 1,4,7,10,13,16-hexaoxacyclooctadecane (1.2 g, 4.56 mmol), and diethyl malonate (9.17 mL, 60.15 mmol) were added to a microwave vial, which was capped and purged with nitrogen for several minutes then heated to 115° C. for 19 h. The reaction was cooled to ambient temperature then water and EtOAc were added. The layers were separated and the aqueous solution was extracted with EtOAc and DCM. The combined organic layers were washed with brine then dried (Na2SO4). The solvent was removed under reduced pressure. Purification (FCC, SiO2, 0-70%, EtOAc/hexanes) afforded the title compound as a pure beige solid (1.76 g, 53.8%). 1H NMR (400 MHz, CDCl3) δ 8.84 (dd, J=18.1, 2.5 Hz, 2H), 8.27 (d, J=1.4 Hz, 1H), 7.68 (d, J=2.6 Hz, 1H), 7.47-7.30 (m, 1H), 7.26-7.17 (m, 2H), 5.20 (s, 2H), 4.22 (q, J=7.2 Hz, 2H), 3.86 (s, 2H), 1.30 (t, J=7.2 Hz, 3H). [M+H]=359.2.

후처리

  1. customwas capped
  2. custompurged with nitrogen for several minutes
  3. temperatureThe reaction was cooled to ambient temperature
  4. additionwater and EtOAc were added
  5. customThe layers were separated
  6. extractionthe aqueous solution was extracted with EtOAc and DCM
  7. washThe combined organic layers were washed with brine
  8. dry with materialthen dried (Na2SO4)
  9. customThe solvent was removed under reduced pressure
  10. customPurification (FCC, SiO2, 0-70%, EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-3ccc568d4355467c9678210b712ea4d6
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09102674B2

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