반응 #55916

반응 방정식

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

수율 44.6%

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

수율 44.6%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도The mixture was cooled in ice
2. 2
   세척after which the solution was washed with water, dilute sodium hydroxide solution and water again
3. 3
   건조dried over magnesium sulphate
4. 4
   기타The crude product was recrystallised from toluene

실험 절차

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.

출처