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Ethanol → (5S)-{4'-[5-(acetylamino-methyl)-2-oxo-oxazolidin-3-yl]-2'-fluoro-biphenyl-4-ylmethyl}-(3-fluoro-propyl)-carbamic acid tert-butyl ester

HRID 2190695
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2190695
C([C:5]([N:7]([CH2:12][C:13]1[CH:18]=[CH:17][C:16](B(O)O)=[CH:15][CH:14]=1)[CH2:8][CH2:9][CH2:10][F:11])=[O:6])(C)(C)C.CC[OH:24].[F:25][C:26]1[CH:27]=[C:28]([N:33]2[CH2:37][C@H:36]([CH2:38][NH:39][C:40](=[O:42])[CH3:41])[O:35][C:34]2=[O:43])[CH:29]=[CH:30][C:31]=1I.C([O-])([O-])=O.[K+].[K+].[C:50]1([CH3:56])[CH:55]=CC=C[CH:51]=1>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>[C:50]([O:24][C:5](=[O:6])[N:7]([CH2:12][C:13]1[CH:14]=[CH:15][C:16]([C:31]2[CH:30]=[CH:29][C:28]([N:33]3[CH2:37][C@H:36]([CH2:38][NH:39][C:40](=[O:42])[CH3:41])[O:35][C:34]3=[O:43])=[CH:27][C:26]=2[F:25])=[CH:17][CH:18]=1)[CH2:8][CH2:9][CH2:10][F:11])([CH3:56])([CH3:55])[CH3:51]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 702EthanolHCID 1140TolueneHCID 11430Potassium CarbonateHCID 11222662(S)-N-[3-(3-Fluoro-4-iodo-phenyl)-2-oxo-oxazolidin-5-ylmethyl]-acetamideHCID 219074294-(N-tert-butylcarbonyl-3-fluoropropylaminomethyl)phenyl boronic acid

Produkt 1

HCID 68540787
(5S)-{4'-[5-(acetylamino-methyl)-2-oxo-oxazolidin-3-yl]-2'-fluoro-biphenyl-4-ylmethyl}-(3-fluoro-propyl)-carbamic acid tert-butyl ester
Ausbeute 30 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418397HCID 178418397, VerbindungKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

A suspension of aryl boronic acid 120 (2.50 g, 8.03 mmol) in a mixture of toluene (24 mL), EtOH (8 mL), and water (8 mL) was treated with aryl iodide 108 (2.53 g, 6.7 mmol, 0.83 equiv) and solid K2CO3 (2.80 g, 20.1 mmol, 3.0 equiv) at room temperature. The resulting reaction mixture was degassed three times under a steady stream of argon before tetrakis(triphenylphosphine)palladium (0) (Pd(PPh3)4, 387 mg, 0.335 mmol, 0.05 equiv) was added. The resulting reaction mixture was degassed three times under a steady stream of argon before being warmed to reflux for 8 h. When TLC and HPLC/MS showed the reaction was complete, the reaction mixture was cooled to room temperature before being poured into water (60 mL) and EtOAc (60 mL). The two layers were separated, and the organic phase was washed with water (30 mL) and saturated aqueous NaCl (2×30 mL), dried over anhydrous Na2SO4, and concentrated in vacuo. The product was then recrystallized from EtOAc/hexanes and dried in vacuo to afford the desired (5S)-{4′-[5-(acetylamino-methyl)-2-oxo-oxazolidin-3-yl]-2′-fluoro-biphenyl-4-ylmethyl}-(3-fluoro-propyl)-carbamic acid tert-butyl ester 121 (1.3 g, 30%) as an off-white powder.

Aufarbeitung

  1. customThe resulting reaction mixture
  2. additionwas added
  3. customThe resulting reaction mixture
  4. customwas degassed three times under a steady stream of argon
  5. temperaturebefore being warmed
  6. temperatureto reflux for 8 h
  7. additionbefore being poured into water (60 mL) and EtOAc (60 mL)
  8. customThe two layers were separated
  9. washthe organic phase was washed with water (30 mL) and saturated aqueous NaCl (2×30 mL)
  10. dry with materialdried over anhydrous Na2SO4
  11. concentrationconcentrated in vacuo
  12. customThe product was then recrystallized from EtOAc/hexanes
  13. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-9362ebce174b40eba24d7e54fb51b334
Quelldatensatz
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08324398B2

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