HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-(5-Chloromethyl-2-n-propoxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo-[4,3-d]pyrimidin-7-one → 1-Methyl-5-(5-methyl-2-n-propoxyphenyl)-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-pyrimidin-7-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-(5-Chloromethyl-2-n-propoxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo-[4,3-d]pyrimidin-7-one | HCID 136116209 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1-Methyl-5-(5-methyl-2-n-propoxyphenyl)-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-pyrimidin-7-one | HCID 135543996 | 27.1% |
Reaction Steps
A solution of 5-(5-chloromethyl-2-n-propoxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one (0.5 g, 0.0013 mol) in ethyl acetate (50 ml) was stirred with 10% palladium on charcoal catalyst under a hydrogen atmosphere at 50 p.s.i. and room temperature. After 1 hour, the mixture was filtered and the filtrate evaporated under vacuum to give a pale green solid. Chromatography on silica gel (4 g) using a methanol in dichloromethane elution gradient gave a white solid, crystallisation of which from hexane-ethyl acetate gave the title compound as colourless needles (0.12 g, 26%), m.p. 115°-116° C. Found: C,66.66; N,7.12; N,16.55. C19H24N4O2 requires C,67.04; H,7.11; N,16.46%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05426107 |
| Source dataset | uspto-grants-1995_06 |
| ORD ID | ord-44c42752cb044a9bb2d25ffb65356aaa |
| Source note | uspto-grants-1995_06 |