Calcium hypochlorite → 6-Chloro-8-difluoromethoxychroman-4-one

HRID 353248Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 353248
[Cl:1][O-].[Ca+2].Cl[O-].[F:6][CH:7]([F:20])[O:8][C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:18]=1[O:17][CH2:16][CH2:15][C:14]2=[O:19]>O.C(O)(=O)C.C(#N)C.O>[Cl:1][C:11]1[CH:12]=[C:13]2[C:18](=[C:9]([O:8][CH:7]([F:6])[F:20])[CH:10]=1)[O:17][CH2:16][CH2:15][C:14]2=[O:19]

Komponenten

6

Edukt 2

HCID 24504Calcium hypochloriteHCID 227083468-Difluoromethoxychroman-4-one

Produkt 1

HCID 227083496-Chloro-8-difluoromethoxychroman-4-oneAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittelHCID 21899381Acetic acid--water (1/1)Lösungsmittel

Versuchsvorschrift

To a solution of calcium hypochlorite (29.4 g, 137.8 mmol) in water:acetic acid (125:9.5) was added a solution of 8-difluoromethoxychroman-4-one (7.4 g, 34.6 mmol, see step (iv) above) in acetonitrile (20 mL), whereafter the reaction mixture was stirred overnight. The mixture was diluted with water and extracted with ether (3×) and with EtOAc (1×). The combined organic layers were washed with water (3×), dried (Na2SO4) and evaporated, yielding 8.0 g (93%) of the subtitle compound.

Aufarbeitung

  1. extractionextracted with ether (3×) and with EtOAc (1×)
  2. washThe combined organic layers were washed with water (3×)
  3. dry with materialdried (Na2SO4)
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-8efa8896b30c49c487ad764f0aac41cd
Quelldatensatz
uspto-grants-2004_06
Patentnummer
US06750243B1

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