تفاعل #1340570

معادلة التفاعل

Bis(4-hydroxyphenyl)phenylsulfonium triflate

potassium nonaflate

→

white solid

المردود 61.0%

Bis(4-hydroxyphenyl)Phenylsulfonium Nonaflate

المردود 61.0%

المذيبات

water

water

ظروف التفاعل

المعالجة

1. 1
   أخرىformed a cloudy solution
2. 2
   أخرىThe formed oil was separated from the aqueous layer
3. 3
   أخرىby decanting this layer away
4. 4
   غسيلThe residual oil was washed with 2 mL of distilled water
5. 5
   workup.DISSOLUTIONThis residue was dissolved in 4 mL acetone
6. 6
   استخلاصThis mixture was then extracted with 100 mL of methylene chloride
7. 7
   workup.STIRRINGafter stirring overnight
8. 8
   غسيلThe methylene chloride layer was washed with water several times
9. 9
   workup.DISSOLUTIONDissolving in a minimum of methylene chloride the residue
10. 10
    أخرىwas precipitated with pentane
11. 11
    أخرىdried under high vacuum

الإجراء التجريبي

Bis(4-hydroxyphenyl)phenylsulfonium triflate (2.5 g, 0.00739 moles; Dainippon Pharmaceuticals) was dissolved in 20 mL of water in a suitable container to which was added potassium nonaflate (3.28 g, 0.00739 mole). To this mixture was added 120 mL of water, which formed a cloudy solution. This solution was stirred overnight at room temperature in a stoppered flask. The formed oil was separated from the aqueous layer by decanting this layer away. The residual oil was washed with 2 mL of distilled water. This residue was dissolved in 4 mL acetone and another 2.6 g of potassium nonaflate and 100 mL of water. This mixture was then extracted with 100 mL of methylene chloride after stirring overnight. The methylene chloride layer was washed with water several times and stripped of solvents. Dissolving in a minimum of methylene chloride the residue was precipitated with pentane and then dried under high vacuum to give 2.68 g of white solid (61% yield) which was pure by 1H and 19F NMR.

المصدر