Reacción #2195499

Ecuación de reacción

product

Diethyl 2,2,4,4,-tetrafluoro-3-oxopentanedioate hydrate

1,3-propanedithiol

→

title compound

Diethyl 2,2′-(1,3-dithiane-2,2-diyl)bis(2,2-difluoroacetate)

Disolventes

methylene chloride

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturacool in an ice/water bath under argon
2. 2
   Filtraciónthen filter
3. 3
   Otrothe reaction
4. 4
   Lavadowashing with ether
5. 5
   workup.ADDITIONAdd 100 mL of ether
6. 6
   Lavadowash with saturated sodium bicarbonate, water, and brine
7. 7
   Secadodry over MgSO4
8. 8
   OtroPurify by silica gel chromatography

Procedimiento

Dissolve 12.1 mmol of the product of Example 6 in 50 mL of methylene chloride and cool in an ice/water bath under argon. Add 6 g of powdered activated 3A molecular sieves, 18.2 mmol of 1,3-propanedithiol, and then 2.4 mmol of BF3Et2O. Stir for 18 h in the cold, then filter the reaction, washing with ether. Add 100 mL of ether and wash with saturated sodium bicarbonate, water, and brine, and dry over MgSO4. Purify by silica gel chromatography using ether/hexane as eluant to yield the title compound.

Fuente