Carbon Dioxide → HCID 54406031, compound

HRID 1580543Notes

Reaction equation

HRID 1580543 reaction equation
C(=O)([O-])[O-].[Na+].[Na+].C(=O)=O.[F:10][C:11]([C:37](F)([F:39])[F:38])([O:15][C:16]([F:36])([F:35])[C:17]([F:34])([C:30]([F:33])([F:32])[F:31])[O:18][C:19]([F:29])([F:28])[C:20]([F:27])([C:25]#[N:26])[C:21]([F:24])([F:23])[F:22])C(F)=O>>[F:38][C:37]([F:39])=[C:11]([F:10])[O:15][C:16]([F:36])([F:35])[C:17]([F:34])([C:30]([F:31])([F:32])[F:33])[O:18][C:19]([F:28])([F:29])[C:20]([F:27])([C:25]#[N:26])[C:21]([F:24])([F:23])[F:22]

Participants

4

Reactant 3

HCID 280Carbon DioxideHCID 10340Sodium CarbonateHCID 53968757HCID 53968757, compound

Product 1

HCID 54406031HCID 54406031, compoundYield 95%

Procedure

A bed (8 × 90 cm) of finely divided dry sodium carbonate held at 250°-270°C. in a vertical glass tube was fluidized with a minimum flow of preheated (300°C.) nitrogen from the bottom, and the exit gases passed out the top and through a series of three dry-ice cooled traps. Perfluoro(8-cyano-2,5-dimethyl-3,6-dioxanonanoyl) fluoride (215 g) was added at 0.59 ml/minute to the preheated nitrogen entering the bed. After all of the acid fluoride had been added, the traps were washed out with the aid of ethyl ether and the combined trap contents distilled to give 172 g (95%) of perfluoro(8-cyano-5-methyl-3,6-dioxa-1-nonene).

Workup

  1. customheld at 250°-270°C. in a vertical glass tube
  2. customwas fluidized with a minimum flow of preheated (300°C.) nitrogen
  3. washthe traps were washed out with the aid of ethyl ether
  4. distillationthe combined trap contents distilled

Sources & evidence

ORD record
ord-2778ebfc96e242e68e223d0aa795171f
Source dataset
uspto-grants-1976_01
Patent number
US03933767

Reaction notes

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