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Boron trifluoride etherate → 2-(9-amino-7-bromo-4-fluoro-2-methoxy-9H-xanthen-9-yl)ethanol

HRID 931594
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 931594
[Br:1][C:2]1[CH:15]=[C:14]2[C:5]([O:6][C:7]3[C:8]([F:19])=[CH:9][C:10]([O:17][CH3:18])=[CH:11][C:12]=3[C:13]2=O)=[CH:4][CH:3]=1.[Cl-].[C:21]([O:25]C(=O)C[Zn+])(C)(C)[CH3:22].[N:30]([Si](C)(C)C)=[N+]=[N-].B(F)(F)F.CCOCC.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1C=CC=CC=1.C1COCC1>[NH2:30][C:13]1([CH2:22][CH2:21][OH:25])[C:12]2[CH:11]=[C:10]([O:17][CH3:18])[CH:9]=[C:8]([F:19])[C:7]=2[O:6][C:5]2[C:14]1=[CH:15][C:2]([Br:1])=[CH:3][CH:4]=2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 8000Boron trifluoride etherateHCID 78378AzidotrimethylsilaneHCID 21226445Aluminium lithium hydrideHCID 574756397-bromo-4-fluoro-2-methoxy-9H-xanthen-9-oneHCID 178451183HCID 178451183, Verbindung

Produkt 1

HCID 67382798
2-(9-amino-7-bromo-4-fluoro-2-methoxy-9H-xanthen-9-yl)ethanol
Ausbeute 48,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 241BenzeneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a suspension of 7-bromo-4-fluoro-2-methoxy-9H-xanthen-9-one (20 g, 61.9 mmol) in 2-methyl-THF (300 mL) a solution of (2-tert-butoxy-2-oxoethyl)zinc(II) chloride (0.5 M in Et2O; 186 mL, 93 mmol) was added at RT. The mixture was stirred for 10 min at RT, and then heated to 45° C. for 1 hour. The reaction mixture was cooled to RT and quenched with aqueous, saturated NH4Cl (150 mL) and water (100 mL). The organic layer was separated, washed with brine and filtered through the pad of Celite. The solvent was removed under reduced pressure to yield as a yellowish solid which was dissolved in of benzene (200 mL). Azidotrimethylsilane (12.30 mL, 93 mmol) was added and the reaction mixture was cooled to 5° C. Borontrifluoride etherate (7.84 mL, 61.9 mmol) was added drop wise. The reaction mixture was quenched by the addition of MeOH (5 mL) and aqueous, saturated NaHCO3 solution (100 ml). The organic layer was separated, washed with brine, filtered through Celite and concentrated under reduced pressure to afford a yellow residue, which was dissolved in THF (300 mL). The solution was cooled to 0° C. and LAH (1M in THF; 93 mL, 93 mmol) was added drop wise at this temperature. The reaction mixture was allowed to warm to RT and quenched by the addition of sodium sulfate decahydrate (20 g). The reaction mixture was stirred for 2 hrs at RT, then filtered through celite. The filter cake was washed twice with EtOAc. The filtrate was concentrated under reduced pressure and the residue was purified by chromatography [5-50% DCM/MeOH/NH4OH (90:10:1)] in DCM to afford 2-(9-amino-7-bromo-4-fluoro-2-methoxy-9H-xanthen-9-yl)ethanol (10.99 g, 29.8 mmol).

Aufarbeitung

  1. additionwas added at RT
  2. temperatureheated to 45° C. for 1 hour
  3. temperatureThe reaction mixture was cooled to RT
  4. customquenched with aqueous, saturated NH4Cl (150 mL) and water (100 mL)
  5. customThe organic layer was separated
  6. washwashed with brine
  7. filtrationfiltered through the pad of Celite
  8. customThe solvent was removed under reduced pressure
  9. customto yield as a yellowish solid which
  10. temperaturethe reaction mixture was cooled to 5° C
  11. customThe reaction mixture was quenched by the addition of MeOH (5 mL)
  12. customThe organic layer was separated
  13. washwashed with brine
  14. filtrationfiltered through Celite
  15. concentrationconcentrated under reduced pressure
  16. customto afford a yellow residue, which
  17. temperatureThe solution was cooled to 0° C.
  18. temperatureto warm to RT
  19. customquenched by the addition of sodium sulfate decahydrate (20 g)
  20. stirringThe reaction mixture was stirred for 2 hrs at RT
  21. filtrationfiltered through celite
  22. washThe filter cake was washed twice with EtOAc
  23. concentrationThe filtrate was concentrated under reduced pressure
  24. customthe residue was purified by chromatography [5-50% DCM/MeOH/NH4OH (90:10:1)] in DCM

Quellen und Nachweise

ORD-Eintrag
ord-44a7090632dc43549570646a2071fa19
Quelldatensatz
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09296759B2

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