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Potassium Phosphate, Tribasic → HCID 86664223, 화합물

HRID 1184484
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HRID 1184484 반응식
P([O-])([O-])([O-])=O.[K+].[K+].[K+].[CH2:9]([B-](F)(F)F)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[K+].Cl[C:22]1[C:27]2[O:28][CH:29]([CH3:33])[C:30](=[O:32])[NH:31][C:26]=2[CH:25]=[C:24]([CH:34]=[O:35])[CH:23]=1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC(C)C)=CC=CC=2OC(C)C)CCCCC1>C1(C)C=CC=CC=1.O.CC(O)C>[CH2:9]([C:22]1[C:27]2[O:28][CH:29]([CH3:33])[C:30](=[O:32])[NH:31][C:26]=2[CH:25]=[C:24]([CH:34]=[O:35])[CH:23]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1
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참가 물질

8

반응물 4

HCID 62657Potassium Phosphate, TribasicHCID 162179852-Dicyclohexylphosphino-2',6'-diisopropoxybiphenylHCID 23692459Potassium benzyltrifluoroboranuideHCID 866642218-Chloro-2-methyl-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-carbaldehyde

생성물 1

HCID 86664223HCID 86664223, 화합물수율 28.2%

시약·촉매·용매 3

HCID 962Water용매2회
HCID 1140Toluene용매
HCID 3776Isopropanol용매

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온도
115 °C

실험 절차

To a suspension of potassium phosphate, tribasic (0.564 g, 2.66 mmol), potassium benzyltrifluoroborate (0.263 g, 1.330 mmol), 8-chloro-2-methyl-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-carbaldehyde 15 (0.2 g, 0.886 mmol) in toluene (Ratio: 5.00, 20 mL) and water (Ratio: 1.000, 4.0 mL) was added PdOAc2 (0.015 g, 0.066 mmol) and dicyclohexyl(2′,6′-diisopropoxybiphenyl-2-yl)phosphine (0.062 g, 0.133 mmol) at 23° C. The reaction was stirred at 115° C. for 20 hr. The reaction mixture was poured into water (2 mL) and extracted with Et2O (3×5 mL). The organic layer was dried over Na2SO4, filtered, and the organic phase stripped to dryness via rotary evaporation. The resulting crude material was reconstituted in DCM (1.0 mL) and purified via medium pressure chromatography using a gradient eluant of 1-5% MeOH:DCM. The appropriate fractions were combined and solvent was removed via rotary evaporation. The late eluting fractions were dried in vacuo to provide a yellow solid. The yellow solid was re-suspended in IPA (1.0 mL), heated at reflux to furnish a solution, cooled to room temperature, filtered, rinsed with IPA, and dried in vacuo to provide the title compound as an off-white solid (0.0704 g, 0.250 mmol, 28.2% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.36 (d, J=6.82 Hz, 3H) 3.98 (s, 2H) 4.75-4.81 (m, 1H) 7.16-7.32 (m, 6H) 7.45 (d, J=2.02 Hz, 1H) 9.80 (s, 1H) 10.93 (s, 1H). ESI-MS: m/z 282.2 (M+H)+. mp=163.2-166.1° C.

후처리

  1. additionwas added
  2. customat 23° C
  3. extractionextracted with Et2O (3×5 mL)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. customthe organic phase stripped to dryness via rotary evaporation
  7. custompurified via medium pressure chromatography
  8. customsolvent was removed via rotary evaporation
  9. washThe late eluting fractions
  10. customwere dried in vacuo
  11. customto provide a yellow solid
  12. temperatureheated
  13. temperatureat reflux
  14. customto furnish a solution
  15. temperaturecooled to room temperature
  16. filtrationfiltered
  17. washrinsed with IPA
  18. customdried in vacuo

출처 및 근거

ORD 기록
ord-70fc821f69d74a2dbf7b00581f7e2830
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08669249B2

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