HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19031029, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Ethoxy-2-methoxybenzoic acid | HCID 18001090 | — |
| Reactant | HCID 18960739 | HCID 18960739 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19031029 | HCID 19031029 | 61.4% |
Reaction Steps
7-Fluoro-1-(4-piperidinyl)-3,4-dihydrocarbostyril (2.37 g), 2-methoxy-4-ethoxybenzoic acid (2.43 g) and bis(2-oxo-oxazolydinyl)phosphinyl chloride (3.65 g) are dissolved in dichloromethane (50 ml) and thereto is added dropwise triethylamine (4 ml). The mixture is stirred at room temperature overnight and poured into water. The mixture is extracted with dichloromethane, dried with sodium carbonate and then purified by silica gel column chromatography (solvent; n-hexane:ethyl acetate=1:1). The resultant is recrystallized from ethanol/water to give 7-fluoro-1-[1-(2-methoxy-4-ethoxybenzoyl)-4-piperidinyl]-3,4-dihydrocarbostyril (2.5 g) as white powder, m.p. 159°-161° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05356904 |
| Source dataset | uspto-grants-1994_10 |
| ORD ID | ord-9bb28b7119aa4c2e921aaafc782c87da |
| Source note | uspto-grants-1994_10 |