Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Trifluoroacetohydrazide | HCID 229753 | — |
| Reactant | Ethyl {2-cyano-1-[4-(trifluoromethyl)phenyl]ethenyl}carbamate | HCID 76754610 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 178517470 | HCID 178517470 | — |
Reaction Steps
2.42 g (8.5 mmol) of ethyl {2-cyano-1-[4-(trifluoromethyl)phenyl]ethenyl}carbamate (Example 129A) and 1.09 g (8.5 mmol) of 2,2,2-trifluoroacetohydrazide are dissolved in NMP (10 ml) and stirred in a flask with a calcium chloride drying tube at an oil-bath temperature of 160° C. for 4 h. The reaction mixture is cooled to RT and ethyl acetate (150 ml) and water (100 ml) are added. The organic phase is separated off, dried with magnesium sulphate and concentrated. The residue is stirred with diethyl ether (25 ml), and the solid is filtered off and dried. 0.67 g (23% of theory) of the product is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08273752B2 |
|---|
| Source dataset | uspto-grants-2012_09 |
|---|
| ORD ID | ord-39287de0c7d445be8dec6a7f27255969 |
|---|
| Source note | uspto-grants-2012_09 |
|---|