Reaktion #55916

Reaktionsgleichung

dichloromethane

4-Hydroxy-3-(2-hydroxy-1,1-dimethylethyl)phenyl methanesulphonate

4-hydroxy-3-(2-hydroxy-1,1-dimethylethyl)phenyl methanesulphonate

triethylamine

ethyl phosphorodichloridate

→

desired product

Ausbeute 44.6%

2-Ethoxy-4,5-dihydro-5,5-dimethyl-2-oxo-1,3,2-benzodioxaphosphepin-7-yl methanesulphonate

Ausbeute 44.6%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was cooled in ice
2. 2
   Waschenafter which the solution was washed with water, dilute sodium hydroxide solution and water again
3. 3
   Trocknendried over magnesium sulphate
4. 4
   SonstigeThe crude product was recrystallised from toluene

Vorschrift

4-Hydroxy-3-(2-hydroxy-1,1-dimethylethyl)phenyl methanesulphonate (10 g) from Example 1 was suspended in acetonitrile (100 ml) and triethylamine (8 g) was added. The mixture was cooled in ice, and ethyl phosphorodichloridate (6.9 g) was added dropwise with vigorous stirring. Stirring was continued for 6 hours prior to the addition of dichloromethane (200 ml), after which the solution was washed with water, dilute sodium hydroxide solution and water again, dried over magnesium sulphate and run down. The crude product was recrystallised from toluene, yielding 6.0 g of the desired product, melting point 113°-115° C.

Quelle