Reaktion #543094

Reaktionsgleichung

potassium carbonate

1,4-dioxa-spiro[4.5]dec-8-yl methanesulphonate

water

potassium carbonate

1,4-dioxa-spiro[4.5]dec-8-yl methanesulphonate

potassium carbonate

1,4-dioxa-spiro[4.5]dec-8-yl methanesulphonate

3-benzyl-6-hydroxy-7-methoxy-3H-quinazolin-4-one

→

3-benzyl-6-(1,4-dioxa-spiro[4.5]dec-8-yloxy)-7-methoxy-3H-quinazolin-4-one

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture is stirred for a further 4 h at 80° C
2. 2
   workup.ADDITIONare very slowly added dropwise
3. 3
   workup.STIRRINGwith stirring, whereupon a precipitate
4. 4
   Sonstigeis formed which
5. 5
   Filtrationfiltered
6. 6
   Waschenwashed with water
7. 7
   Sonstigedried

Vorschrift

20.00 g 3-benzyl-6-hydroxy-7-methoxy-3H-quinazolin-4-one in 150 ml N,N-dimethylformamide are heated to 50° C., then 16.00 g potassium carbonate and 20.00 g 1,4-dioxa-spiro[4.5]dec-8-yl methanesulphonate are added and the reaction mixture is stirred overnight at 80° C. Then another 6.00 g potassium carbonate and 8.00 g 1,4-dioxa-spiro[4.5]dec-8-yl methanesulphonate are added and the mixture is stirred for a further 4 h at 80° C. Within the next 24 h a total of a further 6.00 g potassium carbonate and 10.00 g 1,4-dioxa-spiro[4.5]dec-8-yl methanesulphonate are added batchwise until the reaction is complete. After cooling to ambient temperature a total of 450 ml of water are very slowly added dropwise with stirring, whereupon a precipitate is formed which is suction filtered, washed with water and dried.

Quelle