تفاعل #55916

معادلة التفاعل

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

المردود 44.6%

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

المردود 44.6%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was cooled in ice
2. 2
   غسيلafter which the solution was washed with water, dilute sodium hydroxide solution and water again
3. 3
   تجفيفdried over magnesium sulphate
4. 4
   أخرىThe crude product was recrystallised from toluene

الإجراء التجريبي

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.

المصدر