Reaktion #6373

ord-a8539b47ced44f24996e5458c2287ac2

Reaktionsgleichung

O=C(C(c1ccccc1)c1ccc(O)cc1O)C(c1ccccc1)c1ccc(O)cc1O
2,4-dihydroxy-phenyl-benzyl-ketone
C1COCCN1
morpholine
CCOC([O-])[O-]
ethyl-orthoformate
O=c1c(-c2ccccc2)coc2cc(O)ccc12
7-hydroxy-isoflavone
Ausbeute 91.9%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter 25 minutes crystallization
  2. 2
    workup.ADDITIONAt the end of the reaction time the crystallized suspension is diluted with 120 ml of chloroform and it
  3. 3
    Sonstigeis crystallized at 0° C. for 2 hours
  4. 4
    FiltrationAfter filtration the product
  5. 5
    Sonstigedried

Vorschrift

50 g (0.219 mole) of a mixture of 2,4-dihydroxy-phenyl-benzyl-ketone, 20 ml of dimethyl-formamide, 2.6 ml of morpholine and 39.06 g (0.26 mole) of ethyl-orthoformate is stirred for 7 hours at 80°-90° C. After 25 minutes crystallization can be observed. At the end of the reaction time the crystallized suspension is diluted with 120 ml of chloroform and it is crystallized at 0° C. for 2 hours. After filtration the product is covered twice with 45 ml of chloroform and dried. 47.9 g of 7-hydroxy-isoflavone are obtained.

Quelle

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