HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 19913669, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Azetidine, 1-((10-chloro-4-oxo-3-phenyl-4H-pyrido(2,1-a)phthalazin-1-yl)carbonyl)-3-methoxy- | HCID 3066687 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 19913669 | HCID 19913669 | — |
Reaction Steps
1.26 g of 1-[(10-chloro-4-oxo-3-phenyl-4H-pyrido[2,1-a]phthalazin-1-yl)carbonyl]-3-methoxyazetidine and 0.75 g of sodium cyanoborohydride in 30 ml of methanol are treated dropwise at room temperature under argon with saturated methanolic hydrochloric acid. The reaction is completed after a short time. The mixture is poured into 70 ml of ice-water and the yellowish crystals are removed by filtration. The crystals are washed three times with 2 ml of water each time and dried at 60° in vacuo. After recrystallization of the crude product from ethyl acetate/acetone (1:1), there is obtained 1-[(10-chloro-6,7-dihydro-4-oxo-3-phenyl-4H-pyrido[2,1-a]phthalazin-1-yl)carbonyl]-3-methoxyazetidine as yellowish crystals of m.p. 238°-239°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04889854 |
| Source dataset | uspto-grants-1989_12 |
| ORD ID | ord-21bd9a85f2784eb2b3430534233142cc |
| Source note | uspto-grants-1989_12 |