HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 85916576, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3-(Dimethylamino)-1-propanol | HCID 76646 | — |
| Reactant | HCID 85916602 | HCID 85916602 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 85916576 | HCID 85916576 | — |
Reaction Steps
To a suspension of 3.6 g of sodium hydride in 100 ml of dry benzene 15.3 g of 3-(dimethylamino)propanol are added dropwise at reflux temperature with stirring. Heating is continued for 10 hours. After this time, 34.4 g of 5-chloro-8-ethyl-8H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[3,4-e]-pyrimidine-3-carboxylic acid, ethyl ester are added and the solution is refluxed for 5 additional hours. The solution is evaporated to dryness and the residue is treated with water, filtered off and recrystallized from ethyl acetate. 12 g of 5-[3-(dimethylamino)propoxy]-8-ethyl-8H-pyrazolo-[1,5-a]pyrazolo[4',3':5,6]pyrido[3,4-e]pyrimidine-3-carboxylic acid, ethyl ester are obtained (29.3%); m.p. 106°-107°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04233300 |
| Source dataset | uspto-grants-1980_11 |
| ORD ID | ord-9d40a78361454d97aa4ac9443912bad0 |
| Source note | uspto-grants-1980_11 |