HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,8-Diazabicyclo(5.4.0)undec-7-ene → 1-Ethyl-6-fluoro-7-(3-methyl-3,8-diazaspiro[4.4]nonan-8-yl)-4-oxo-1,8-naphthyridine-3-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | 7-Chloro-1-ethyl-6-fluoro-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylic acid | HCID 12790859 | — |
| Reactant | 2-Methyl-2,7-diazaspiro[4.4]nonane dihydrochloride | HCID 13491806 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1-Ethyl-6-fluoro-7-(3-methyl-3,8-diazaspiro[4.4]nonan-8-yl)-4-oxo-1,8-naphthyridine-3-carboxylic acid | HCID 461885 | 53.3% |
Reaction Steps
A stirred suspension of 4.40 g (20.7 mmol) of 2-methyl-2,7-diazaspiro[4.4]nonane dihydrochloride in 200 ml acetonitrile was treated with 9.42 g (62 mmol) 1,8-diazabicyclo[5.4.0]undec-7-ene and 5.42 g (20 mmol) 1-ethyl-6-fluoro-7-chloro-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylic acid was added. After stirring 23 hours at room temperature the precipitated product was filtered, washed with acetonitrile and ether, and recrystallized from ethanol to afford 3.99 g of the title compound, mp 252°-254° C. (dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04665079 |
| Source dataset | uspto-grants-1987_05 |
| ORD ID | ord-7d5a92ab0fe84e59b07bf1c711f7e402 |
| Source note | uspto-grants-1987_05 |