Reaktion #6374

ord-90f5082eeee942519d56cfae78d6b65a

Reaktionsgleichung

O=C(C(c1ccccc1)c1ccc(O)cc1O)C(c1ccccc1)c1ccc(O)cc1O
2,4-dihydroxy-phenyl-benzyl-ketone
CCOC([O-])[O-]
ethyl-orthoformate
C1COCCN1
morpholine
O=c1c(-c2ccccc2)coc2cc(O)ccc12
7-hydroxy-isoflavone
Ausbeute 90.6%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeCrystallization
  2. 2
    Temperaturafter heating for 25 minutes
  3. 3
    SonstigeThe inert temperature falls back to 87° C. from 96° C. during the reaction
  4. 4
    workup.STIRRINGAfter stirring for 5 hours the reaction mixture

Vorschrift

A mixture of 20 g (0.0877 mole) 2,4-dihydroxy-phenyl-benzyl-ketone, 20.7 g (0.14 mole) ethyl-orthoformate and 1 ml of morpholine is stirred on a hot water bath. Crystallization starts after heating for 25 minutes. The inert temperature falls back to 87° C. from 96° C. during the reaction. After stirring for 5 hours the reaction mixture is diluted with 48 ml of chloroform and then one may proceed as disclosed in Example 5. 18.9 g of 7-hydroxy-isoflavone are obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05247102uspto-grants-1993_09