HuagongsheHuagongshe Chemistry Print Report · For research reference only
P-Chloroacetophenone → HCID 15338017, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | P-Chloroacetophenone | HCID 7467 | — |
| Reactant | Acetic acid, 2-chloro-2,2-difluoro-, ethyl ester | HCID 67843 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 15338017 | HCID 15338017 | 92.4% |
Reaction Steps
38 g of ethyl chlorodifluoroacetate was added to 22.7 g of sodium methoxide and 300 ml of dry ether under cooling with ice. 31 g of p-chloroacetophenone was gradually added thereto under cooling with ice. The mixture was stirred at room temperature for 12 hours. The solvent was distilled off. 150 ml of 6N hydrochloric acid was added under cooling with ice, and extraction with ethyl acetate was carried out. The extract layer was washed with water, and the solvent was distilled off. The resulting crude product was purified by silica gel column chromatography (developing solvent: chloroform), and thereby 49.5 g of the desired product was obtained as a pale yellow viscous liquid. m.p. 50°-51° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05773388 |
| Source dataset | uspto-grants-1998_06 |
| ORD ID | ord-88dd58538f20473d98d45e69d9e2e91e |
| Source note | uspto-grants-1998_06 |