HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 135979303, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 4-Methoxyphenylacetyl chloride | HCID 2734688 | — |
| Reactant | HCID 54459581 | HCID 54459581 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 135979303 | HCID 135979303 | 75.2% |
Reaction Steps
In 80 ml of benzene was dissolved 10.4 g of N'-cyclopropylmethyloxy-2-fluoro-6-trifluoromethylbenzamidine, and to the solution was added 8.9 g of 4-methoxyphenylacetylchloride. The solution was heated under refluxing for 3 hours. After cooling, ethyl acetate was added to the solution, followed by washing with water and drying over anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure and the residue obtained in crystal was washed with a mixed solvent hexane and ether to thereby obtain 13.7 g of crude crystal. The crystal was then re-crystallized in hexane, thereby affording 11.5 g of the objective compound.m.p. 88-90° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05942538 |
| Source dataset | uspto-grants-1999_08 |
| ORD ID | ord-0218c766caab498592607a8b1d16aace |
| Source note | uspto-grants-1999_08 |