HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Hydroxypyrrolidine → HCID 13520242, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Hydroxypyrrolidine | HCID 98210 | — |
| Reactant | HCID 13373748 | HCID 13373748 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 13520242 | HCID 13520242 | 22.5% |
Reaction Steps
4 ml of dimethyl sulfoxide and 100 mg of 3-hydroxypyrrolidine were added to 100 mg of 8,9-difluoro-5-methylene-1-oxo-6,7-dihydro-1H,5H-benzo(ij)quinolizine-2-carboxylic acid and the resulting mixture was allowed to react for 2 hours at 120° C. The solvent was distilled off. The residue was purified by silica gel column chromatography and purified by preparative thin layer chromatography on silica gel and then recrystallized from a mixture of ethanol and chloroform to give 28 mg of 9-fluoro-8-(3-hydroxy-1-pyrrolidinyl)-5-methylene-1-oxo-6,7-dihydro-1H,5H-benzo(ij)quinolizine-2-carboxylic acid as microcrystals with mp 190°-196° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04535161 |
| Source dataset | uspto-grants-1985_08 |
| ORD ID | ord-a094037dd0434397939cc89317d5c1b8 |
| Source note | uspto-grants-1985_08 |