HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Chloro-4-(chloromethyl)benzene → HCID 13384258, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Chloro-4-(chloromethyl)benzene | HCID 7723 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 13384220 | HCID 13384220 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 13384258 | HCID 13384258 | — |
Reaction Steps
Ethyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate (12.0 g.) is added dropwise at ambient temperature to a stirred mixture of sodium hydride (2.4 g. of a 60% dispersion in oil) and dimethylformamide (100 ml.). The mixture is stirred for 4 hours, 4-chlorobenzyl chloride (8.4 g.) is added, and the stirring is continued for 6 days. The mixture is filtered, and the filtrate is evaporated in vacuo. The residue is fractionally distilled at 0.1 mm. pressure, collecting the fraction, (9.9 g.) b.p. 78°-80° C., m.p. 32°-33° C, which is crystallized from pentane to give ethyl 2-(4-chlorobenzyloxy)-3,3,3-trifluoro-2-trifluoromethylpropionate, m.p. 33° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04055595 |
| Source dataset | uspto-grants-1977_10 |
| ORD ID | ord-21089d16163d49eaa19ca56703c7f452 |
| Source note | uspto-grants-1977_10 |