Acetic Anhydride → HCID 54174825, compound

HRID 964904Notes

Reaction equation

HRID 964904 reaction equation
[Cl:1][C:2]([F:10])([F:9])[C:3](=[O:8])[CH2:4][C:5](=[O:7])[CH3:6].[CH:11]([O-])([O-])[O:12][CH2:13][CH3:14].C(OC(=O)C)(=O)C>O>[Cl:1][C:2]([F:10])([F:9])[C:3](=[O:8])[C:4](=[CH:11][O:12][CH2:13][CH3:14])[C:5](=[O:7])[CH3:6]

Participants

5

Reactant 3

HCID 7918Acetic AnhydrideHCID 27364921-chloro-1,1-difluoropentane-2,4-dioneHCID 53630039Ethylorthoformate

Product 1

HCID 54174825HCID 54174825, compoundYield 48.5%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

A mixed solution containing 50 g of 1-chloro-1,1-difluoro-2,4-pentanedione, 60 g of ethyl orthoformate and 82 g of acetic anhydride was refluxed with stirring for 2 hours. After a Dean-Stark apparatus (water separator) was fixed, the solution was refluxed for additional 4 hours, while about 100 ml of water was removed. After it was allowed to cool, vacuum distillation was conducted to obtain 32.2 g of the desired product as a pale red liquid. Boiling point 95°-118° C./1.6 mmHg.

Workup

  1. temperaturewas refluxed
  2. customwas removed
  3. temperatureto cool
  4. distillationvacuum distillation

Sources & evidence

ORD record
ord-8a0a3598a9ae48ddb158dfc3453166fb
Source dataset
uspto-grants-1998_06
Patent number
US05773388

Reaction notes

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