HCID 12010406, compound → HCID 12010407, compound

HRID 1280113Notes

Reaction equation

HRID 1280113 reaction equation
Cl[C:2]([F:21])([F:20])[C:3](Cl)([F:18])[O:4][C:5]([Cl:17])([F:16])[C:6]([F:15])([F:14])[C:7](Cl)([F:12])[C:8](Cl)([F:10])[F:9]>[Zn].CN(C)C=O>[C:8](=[C:7]([C:6]([C:5]([O:4][C:3](=[C:2]([F:20])[F:21])[F:18])([Cl:17])[F:16])([F:15])[F:14])[F:12])([F:10])[F:9]

Participants

4

Reactant 1

HCID 12010406HCID 12010406, compound

Product 1

HCID 12010407HCID 12010407, compoundYield 60%

Reagents, catalysts & solvents 2

HCID 23994ZincCatalystHCID 6228DimethylformamideSolvent

Procedure

Into a 500 ml four-necked flask equipped with a stirrer, a reflux condenser and a dropping funnel, 120 g (1.84 mol) of zinc was introduced, and 200 ml of dimethylformamide was introduced thereinto in an atmosphere of an inert gas. Then, the pressure in the system was reduced to 4 kPa, and the internal temperature was adjusted to from 50 to 55° C., and 100 g (0.23 mol) of CF2ClCFClCF2CFClOCFClCF2Cl was dropwise added thereto gradually by the dropping funnel, and the resulting product was quickly taken out by distillation during the reaction. Then, the crude product was purified to obtain 39 g (yield 60%) of pure CF2═CFCF2CFClOCF═CF2 (4-chloro-1,1,2,4,5,5,6,7,7-nonafluoro-3-oxa-1,6-heptadiene). Hereinafter this compound will be referred to as a monomer B.

Workup

  1. customInto a 500 ml four-necked flask equipped with a stirrer, a reflux condenser and a dropping funnel
  2. additionwas dropwise added
  3. distillationgradually by the dropping funnel, and the resulting product was quickly taken out by distillation during the reaction
  4. customThen, the crude product was purified

Sources & evidence

ORD record
ord-4a4fe2f9ce71407a901885a35ccc74a7
Source dataset
uspto-grants-2002_09
Patent number
US06448452B2

Reaction notes

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