反応 #55916

反応方程式

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

収率 44.6%

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

収率 44.6%

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度The mixture was cooled in ice
2. 2
   洗浄after which the solution was washed with water, dilute sodium hydroxide solution and water again
3. 3
   乾燥dried over magnesium sulphate
4. 4
   その他The crude product was recrystallised from toluene

実験手順

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.

出典