HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → o-Desethyl sildenafil
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | Demethylpiperazinyl Desethyl Sildenafil Sulfonyl Chloride | HCID 135738545 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | o-Desethyl sildenafil | HCID 135565516 | 97% |
Reaction Steps
A solution of 5-(5-chlorosulphonyl-2-hydroxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one (0.235 g, 0.0006 mol) and N-methylpiperazine (0.5 ml, 0.0045 mol) in ethanol (40 ml) was stirred at room temperature for 18 hours. The solution was evaporated under vacuum and the residue partitioned between ethyl acetate (40 ml) and water (40 ml). The fine precipitate was filtered off, washed with water then ethyl acetate, and crystallised from ethyl acetate/DMF to give the title compound as an off-white powder (0.260 g, 49%), m.p. 283°-284° C. Found: C,53.53; H,5.89; N,18.40. C20H26N6O4S requires C,53.80; H,5.87; N,18.82%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05719283 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-28a324e4858245338e0ecfddecece32e |
| Source note | uspto-grants-1998_02 |