Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phosphoric Acid | HCID 1004 | — |
| Reactant | Phosphorus trichloride | HCID 24387 | — |
| Reactant | 3,4-dihydro-2H-pyrido(1,2-a)pyrimidin-2-one | HCID 79500 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 9948054 | HCID 9948054 | — |
Reaction Steps
5 g 3,4-Dihydropyrido-(1,2-a)-pyrimidin-2-one (Fluka) were melted at 80° C. with 5.5 g H3PO4 and mixed, while stirring, with 5.9 ml PCl3. After 20 hours at the given temperature, it was mixed with 70 ml 2N HCl, stirred for 8 hours at 100° C. and, after cooling, filtered off from the undissolved part. The filtrate was evaporated on a rotary evaporator and purified by ion exchanger chromatography on Amberlite IR 120 (H+ form) with water as eluent. The fractions obtained after electrophoresis were evaporated in a vacuum and the oil remaining behind, after dissolving in a little water, brought to crystallisation by the addition of acetone.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05366969 |
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| Source dataset | uspto-grants-1994_11 |
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| ORD ID | ord-d0c17a9469564c4e942518a3886b630a |
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| Source note | uspto-grants-1994_11 |
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