Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 86761699 | HCID 86761699 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86761698 | HCID 86761698 | — |
Reaction Steps
To a solution of 4.28 g of 3-[3-bromo-5-(trifluoromethyl)phenyl]-1-(3-chloro-4-methylphenyl)-4,4,4-trifluoro-3-hydroxybutane-1-one in 10 mL of toluene, 2.08 g of thionyl chloride and 1.38 g of pyridine were added while stirring the solution at 80° C. to continue the stirring of the resultant mixture at the same temperature for 2 hours. After the completion of the reaction, 10 mL of water was added to the reaction mixture while ice-cooling the reaction mixture and the stirring of the reaction mixture was continued until the temperature of the reaction mixture returned to room temperature. The organic phase was separated off and charged into a solution of 0.77 g of sodium hydroxide in 5 mL of water. The resultant mixture was stirred at room temperature for 30 minutes. The organic phase was separated off and then was dehydrated and dried over saturated saline and anhydrous magnesium sulfate in this order. The solvent was distilled off under reduced pressure to obtain 4.02 g of a crude objective substance as a yellow oily substance. This substance was used in the next process as it was without being further purified.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08318757B2 |
|---|
| Source dataset | uspto-grants-2012_11 |
|---|
| ORD ID | ord-a8fe20077a95429288a0b4ef3d887709 |
|---|
| Source note | uspto-grants-2012_11 |
|---|