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

HRID 1294480Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1294480
[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 sub-title 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-cdf94016d21d4f8bbccb56f6417e469e
Quelldatensatz
uspto-grants-2007_07
Patentnummer
US07241757B2

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