HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 18694241, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 18694229 | HCID 18694229 | — |
| Product | HCID 18694241 | HCID 18694241 | 50% |
Reaction Steps
Crude 4'-amino-2'-trifluoromethylbiphenyl-4-carboxylic acid (D33, 0.31 g, 0.078 mol) was dissolved in methanol (200 ml) and treated with conc. H2SO4 acid (1 ml). The mixture was heated at reflux under argon for 2 hrs, then concentrated in vacuo. The resultant yellow solid was basified with 10% aqueous Na2CO3 solution, extracted with dichloromethane, then the extract dried (Na2SO4) and concentrated in vacuo. The resultant yellow solid was purified by preparative TLC on silica gel plates eluting with 1:1 pet ether/ether to afford the title compound as an off-white solid (161 mg, 50%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06100272 |
| Source dataset | uspto-grants-2000_08 |
| ORD ID | ord-672b62354b0447eeb3594a6b22b5aa1f |
| Source note | uspto-grants-2000_08 |