Pyridine → Hexamethyldisiloxane

HRID 1939614Notes

Reaction equation

HRID 1939614 reaction equation
N1C=CC=CC=1.C([O-])([O-])=O.[Ca+2].[CH3:12][Si:13](F)([CH3:15])[CH3:14].C(O)=O.[OH2:20]>>[CH3:12][Si:13]([CH3:15])([CH3:14])[O:20][Si:13]([CH3:15])([CH3:14])[CH3:12]

Participants

5

Reactant 4

HCID 1049PyridineHCID 9869Fluorotrimethylsilane2×HCID 10112Calcium CarbonateHCID 18673298Formic acid--water (1/1)

Product 1

HCID 24764Hexamethyldisiloxane

Procedure

Working up of the HF/pyridine reaction solution takes place suitably with a suspension of excess finely powdered CaCO3 in ice water with vigorous stirring and filtration of the resultant calcium fluoride. Further, excess hexamethyldisiloxane can be added to the crude reaction mixture with vigorous stirring, so that the phases are at least somewhat mixed, and the volatile trimethylsilyl fluoride (boiling point 17° C.) and water format temperatures between -20° C. and 24° C. The trimethylsilyl fluoride can be cleaved in a receiver with alkaline solution to form alkali fluorides and hexamethyldisiloxane. The working up with hexamethyldisiloxane is particularly suitable for the reaction of the 5'-phosphates.

Workup

  1. filtrationfiltration of the resultant calcium fluoride
  2. additionFurther, excess hexamethyldisiloxane can be added to the crude
  3. customreaction mixture with vigorous stirring
  4. additionsomewhat mixed

Sources & evidence

ORD record
ord-c9c4c516a31b4ad1bc1b9fbbb4d8a0dc
Source dataset
uspto-grants-1997_12
Patent number
US05696255

Reaction notes

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