Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Methanesulfonate | HCID 85257 | — |
| Reactant | HCID 136138673 | HCID 136138673 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 136197590 | HCID 136197590 | 49.7% |
Reaction Steps
Morpholine (0.19 g, 0.0021 mol) was added to a solution of the above mesylate, namely 5-[5-(2-methanesulphonyloxyethoxymethyl)-2-n-propoxyphenyl]-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-pyrimidin-7-one, (0.20 g, 0.00042 mol) in acetonitrile (25 ml) and the stirred mixture was heated under reflux for 18 hours. The solvent was removed by evaporation under vacuum, the residue dissolved in saturated aqueous sodium carbonate solution and the solution extracted with ethyl acetate (3×20 ml). The extracts were combined, dried (Na2SO4) and evaporated under vacuum, and the residue was chromatographed on silica gel (4g) using an elution gradient of methanol in dichloromethane (0-2% methanol). Evaporation under vacuum of the appropriate fractions, followed by crystallisation from hexane, gave the title compound as white crystals (0.098 g, 48%), m.p. 65°-66° C. Found C,64.17; H,7.69; N,14.96. C25H35N5O5 requires C,63.94; H,7.51; N,14.91%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05272147 |
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| Source dataset | uspto-grants-1993_12 |
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| ORD ID | ord-0f758a6e357d493e8c70fde90e71f08c |
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| Source note | uspto-grants-1993_12 |
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