HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 21467012, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Phthalic Anhydride | HCID 6811 | — |
| Reactant | HCID 21467017 | HCID 21467017 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 21467012 | HCID 21467012 | 89.8% |
Reaction Steps
A mixture of 1.62 g of 4-acetoxytetrahydrofuran-3-yl 2-[(5-amino-2-chloro-4-fluorophenyl)amino]propionate, 0.80 g of phthalic anhydride, and 10 ml of acetic acid was heated under reflux for 3 hours while stirring. Water was added to the reaction mixture, and the semi-solid formed was collected by filtration, dissolved in ethyl acetate, washed successively with a saturated aqueous solution of sodium hydrogencarbonate and a saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate-hexane=2:3) to give 1.98 g of the title compound (Table 1, Compound No. 32).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05696056 |
| Source dataset | uspto-grants-1997_12 |
| ORD ID | ord-6b5681823a1d486ab6cb813094190c7f |
| Source note | uspto-grants-1997_12 |