Sulfuric Acid → HCID 18931712, compound

HRID 1599193Notes

Reaction equation

HRID 1599193 reaction equation
S(=O)(=O)(O)O.[Cl:6][C:7]([C:13]([O:21][CH2:22][CH3:23])([O:18][CH2:19][CH3:20])[C:14]([F:17])([F:16])[F:15])=[C:8](F)OCC>C(O)C>[Cl:6][CH:7]([C:13]([O:18][CH2:19][CH3:20])([O:21][CH2:22][CH3:23])[C:14]([F:15])([F:16])[F:17])[CH2:8][C:13]([O:18][CH2:19][CH3:20])=[O:21]

Participants

4

Reactant 2

HCID 1118Sulfuric AcidHCID 53894330HCID 53894330, compound

Product 1

HCID 18931712HCID 18931712, compoundYield 151.8%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

100 ml of 50% strength sulfuric acid were added to 100 g of 2-chloro-I,4,4,4-tetrafluoro-1,3,3-triethoxy-but-1-ene in 200 ml of ethanol and the mixture was stirred under reflux for 3 hours. It was poured onto water and extracted with methylene chloride. The organic phase was dried over sodium sulfate and the solvent was removed in vacuo. The residue was distilled in vacuo. 79 g of ethyl 2-chloro-4,4,4-trifluoro-3,3-diethoxybutanecarboxylate of boiling point 48° C. under 0.2 mbar were isolated.

Workup

  1. temperatureunder reflux for 3 hours
  2. additionIt was poured onto water
  3. extractionextracted with methylene chloride
  4. dry with materialThe organic phase was dried over sodium sulfate
  5. customthe solvent was removed in vacuo
  6. distillationThe residue was distilled in vacuo

Sources & evidence

ORD record
ord-7c655642e2a04875a8b6723aed153a4f
Source dataset
uspto-grants-1998_04
Patent number
US05739394

Reaction notes

Loading…