Potassium Carbonate → 2-(2,4-Difluorophenyl)oxirane

HRID 880617

Reaktionsgleichung

Reaktionsgleichung von HRID 880617
[BH4-].[Na+].Br[CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][C:8]=1[F:14])=[O:6].C([O-])([O-])=O.[K+].[K+]>CO>[F:14][C:8]1[CH:9]=[C:10]([F:13])[CH:11]=[CH:12][C:7]=1[CH:5]1[CH2:4][O:6]1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 27741852-Bromo-2',4'-difluoroacetophenoneHCID 4311764Sodium borohydride

Produkt 1

HCID 143729242-(2,4-Difluorophenyl)oxirane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Sodium borohydride (0.367 g, 10.85 mmol) was added to a stirred solution of 2-bromo-2′,4′-difluoroacetophenone ([CAS 102429-07-2], 5.1 g, 21.7 mmol) in MeOH (152 mL) at 10° C. The mixture was stirred at RT for 1 h. Then, K2CO3 (4.499 g, 32.55 mmol) was added and the mixture was stirred at RT for 1 h. The mixture was filtered through diatomaceous earth and the filtrate was concentrated in vacuo. The residue was treated with water and extracted with CH2Cl2/THF. The organic layer was separated, dried (Na2SO4), filtered and the solvents evaporated in vacuo to yield I-19 (2.24 g, 66%) as a yellow oil.

Aufarbeitung

  1. stirringthe mixture was stirred at RT for 1 h
  2. filtrationThe mixture was filtered through diatomaceous earth
  3. concentrationthe filtrate was concentrated in vacuo
  4. additionThe residue was treated with water
  5. extractionextracted with CH2Cl2/THF
  6. customThe organic layer was separated
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. customthe solvents evaporated in vacuo
  10. customto yield I-19 (2.24 g, 66%) as a yellow oil

Quellen und Nachweise

ORD-Eintrag
ord-cda5a70adcba496dbcc8fc946b69d1c3
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08993591B2

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