反応 #2195499

反応方程式

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)

溶媒

methylene chloride

反応条件

後処理

1. 1
   温度cool in an ice/water bath under argon
2. 2
   ろ過then filter
3. 3
   その他the reaction
4. 4
   洗浄washing with ether
5. 5
   workup.ADDITIONAdd 100 mL of ether
6. 6
   洗浄wash with saturated sodium bicarbonate, water, and brine
7. 7
   乾燥dry over MgSO4
8. 8
   その他Purify by silica gel chromatography

実験手順

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.

出典