HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 15057661, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 67899874 | HCID 67899874 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 15057661 | HCID 15057661 | — |
Reaction Steps
6.86 g (15 mmol) of 5-fluoro-2-hydroxy-3-(trifluoromethyl)-benzoic acid-[2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-ethylamide] is dissolved in 30 ml of methanol, 30 ml of water and 300 mg of cation exchanger Amberlyst 15 are added and refluxed for 2 hours. The ion exchanger is then filtered off, 250 mg of palladium-carbon (10%) is added to the filtrate and hydrogenated for 1 hour at normal pressure. The catalyst is then filtered off, the filtrate is evaporated to dryness in a vacuum and the residue is chromatographed on silica gel 60 (Merck) with dichloromethane/methanol. 3.08 mg (9.41 mmol)=62.7% of the theoretical yield of the compound is obtained as an amorphous solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05130119 |
| Source dataset | uspto-grants-1992_07 |
| ORD ID | ord-56743e1916884a2990195c13711476ff |
| Source note | uspto-grants-1992_07 |