HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzene → HCID 21831322, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 21831314 | HCID 21831314 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 21831322 | HCID 21831322 | 69.5% |
Reaction Steps
A mixture of 0.13 g of 2,2-bisfluoromethyl-6-nitro-4-(1,2-dihydro-2-oxo-1-pyridyl)-2H-1-benzopyran, 83 mg of a Lawesson's reagent, 1 ml of benzene and 1 ml of 1,2-dichloroethane was refluxed for 3 hours and the solvent was distilled off. The resultant residue was purified using silica gel column chromatography (developing solution, CH2Cl2), and then, recrystallized from a mixture of ethyl acetate and hexane to obtain 0.05 g of 2,2-bisfluoromethyl-6-nitro-4-(1,2-dihydro-2-thioxo-1-pyridyl)-2H-1-benzopyran represented by the following formula having a melting point of 209°-210° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05874446 |
| Source dataset | uspto-grants-1999_02 |
| ORD ID | ord-b2bd58d0a45144a0a2881de30edadfe5 |
| Source note | uspto-grants-1999_02 |