Реакция #2195499

Уравнение реакции

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)

Растворители

methylene chloride

Условия реакции

Обработка

1. 1
   Температураcool in an ice/water bath under argon
2. 2
   Фильтрацияthen filter
3. 3
   Другоеthe reaction
4. 4
   Промывкаwashing with ether
5. 5
   workup.ADDITIONAdd 100 mL of ether
6. 6
   Промывкаwash with saturated sodium bicarbonate, water, and brine
7. 7
   Сушкаdry over MgSO4
8. 8
   ДругоеPurify by silica gel chromatography

Методика

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.

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