HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylformamide → 2-trifluoromethyl-7-(N-ethyl-N-formylamino)-6,7,8,9-tetrahydro-[5H]-benzocycloheptene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylformamide | HCID 12319 | — |
| Reactant | 2-trifluoromethyl-6,7,8,9-tetrahydro-[5H]-benzocyclohepten-7-one | HCID 11345199 | — |
| Solvent | Formic Acid | HCID 284 | — |
| Product | 2-trifluoromethyl-7-(N-ethyl-N-formylamino)-6,7,8,9-tetrahydro-[5H]-benzocycloheptene | HCID 14502065 | 99.2% |
Reaction Steps
A mixture of 228.2 g of 2-trifluoromethyl-6,7,8,9-tetrahydro-[5H]-benzocyclohepten-7-one, 219 g of N-ethylformamide and 151 g of formic acid is heated under reflux for 14 hours. After concentration in vacuo, while heating on a bain-marie, the residue is taken up in 2300 ml of methylene chloride. After washing twice with 800 ml of water each time, the organic layer is dried over magnesium sulphate and, after filtration, the solvent is removed in vacuo. 283 g of 2-trifluoromethyl-7-(N-ethyl-N-formylamino)-6,7,8,9-tetrahydro-[5H]-benzocycloheptene are obtained in the form of an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05079245 |
| Source dataset | uspto-grants-1992_01 |
| ORD ID | ord-d6be2dfc797d4afb9d42f33063c4756f |
| Source note | uspto-grants-1992_01 |