HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-Chlorophenyl-2,2-difluoroethanoyl chloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | Ethyl 2-(4-Chlorophenyl)-2,2-difluoroacetate | HCID 21468011 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-Chlorophenyl-2,2-difluoroethanoyl chloride | HCID 23365731 | — |
Reaction Steps
Ethyl 4-chlorophenyl-2,2-difluoroacetate (250 mg) and potassium hydroxide (300 mg) were mixed in 27 ml of ethanol and 2.4 ml of water and the reaction mixture was refluxed for four hours. The mixture was then acidified and extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous Na2SO4 and the solvent was removed in vacuo to give a product which was dissolved in 410 mg of oxalyl chloride with catalytic amount of N,N-dimethylformamide. The mixture was stirred for two hours and excess oxalyl chloride was removed in vacuo to give 4-chlorophenyl-2,2-difluoroethanoyl chloride which was used as is for the subsequent step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05583147 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-9d89a6169e5d4978bb818869452df78f |
| Source note | uspto-grants-1996_12 |