HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 13745628, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 13745623 | HCID 13745623 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 13745628 | HCID 13745628 | — |
Reaction Steps
A mixture of 4-[3-(4-acetyl-3-hydroxy-2-propylphenoxy)propoxy]-3-fluorobenzoic acid (700 mg), dichloromethane (25 ml), triethylamine (2ml), acetic anhydride (2ml) and 4-dimethylaminopyridine (catalytic amount) was stirred at ice-cooling to room temperature for 6.5 hours. To the reaction mixture was added methanol (2ml), and the mixture was stirred for 30 minutes. After concentration, water was added to the residue. Solid materials were recovered by filtration and subjected to recrystallization from aqueous methanol to give crystals of 4-[3-(3-acetoxy-4-acetyl-2-propylphenoxy)propoxy]-3-fluorobenzoic acid (723 mg). m.p. 144°-145° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04714774 |
| Source dataset | uspto-grants-1987_12 |
| ORD ID | ord-707980c8c2ec48f08bc4c32c0c936e17 |
| Source note | uspto-grants-1987_12 |