2-Bromoethanol → HCID 68422485, compound

HRID 730251Notes

Reaction equation

HRID 730251 reaction equation
[C:1]([CH:5]([OH:7])[OH:6])([F:4])([F:3])Cl.Br[CH2:9][CH2:10]O.[Cl-:12].[Ca+2].[Cl-].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:12][C:5]1([CH:1]([F:4])[F:3])[O:7][CH2:10][CH2:9][O:6]1

Participants

6

Reactant 4

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 1129841,1-Ethanediol, 2-chloro-2,2-difluoro-HCID 5284359Calcium Chloride

Product 1

HCID 68422485HCID 68422485, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Conditions

Temperature
90 °C

Procedure

157 g (1.4 mole or less) of CClF2CH(OH)2, 197 g (1.5 mole) of 2-bromoethanol and 20 g of calcium chloride were placed in a 1 liter-sized flask with a condenser. The flask was heated at 90° C. for 7 hours and cooled to room temperature. The upper phase was transferred to a 5 liter-sized flask, and 2 liters of acetone and 386 g (2.8 moles) of potassium carbonate were added to the flask. The mixture was reacted at 50° C. for three days, and a solid was precipitated. The solvent was removed by distillation. The product was purified by distillation. The yield of the product was 88% (195 g) and has a boiling point of 62° C./30 mmHg.

Workup

  1. temperaturecooled to room temperature
  2. customThe mixture was reacted at 50° C. for three days
  3. customa solid was precipitated
  4. customThe solvent was removed by distillation
  5. distillationThe product was purified by distillation

Sources & evidence

ORD record
ord-5dcfad23fe58411a99be1bf20713285e
Source dataset
uspto-grants-2009_09
Patent number
US07582714B2

Reaction notes

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