HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 9946396, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | 1,2-Diaminocyclohexane, trans- | HCID 43806 | — |
| Reactant | HCID 12017607 | HCID 12017607 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 9946396 | HCID 9946396 | 41.8% |
Reaction Steps
A mixture of 1-(4-fluorophenyl)-3-oxo-1,3-dihydro-2-benzofuran-1-carboxamide (5 g) (Step 1 of Example 2), trans 1,2-diaminocyclohexane (8.3 g), and toluene (75 mL) was heated at reflux for 66 h in a flask equipped with a water separator. The mixture was evaporated to dryness and the residual gum was extracted with hexane. The residue was chromatographed over silica gel and eluted with 10% methanol in methylene. Crystallization from ethyl acetate afforded the title compound (2.7 g) as a white solid m.p. 203-205° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06448255B1 |
| Source dataset | uspto-grants-2002_09 |
| ORD ID | ord-97edcc2a865941cdb72f40deefd1c68c |
| Source note | uspto-grants-2002_09 |