Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Oxalate | HCID 71081 | — |
| Reactant | HCID 19898742 | HCID 19898742 | — |
| Reactant | HCID 19898743 | HCID 19898743 | — |
| Reactant | HCID 67794760 | HCID 67794760 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 54319410 | HCID 54319410 | 55% |
Reaction Steps
In 5 ml of N,N-dimethylformamide, reaction was carried out at 90° C. for 1 hour among 0.68 g of 1,3-dimethyl-6-[2-(2-hydroxyethylamino)ethylamino]-2,4-(1H,3H)-pyrimidinedione (Compound 15), 0.96 g of 3-(2-phenyl-3-methyl-4-oxo-4H-1-benzopyran-5-yl)oxypropyl bromide (Compound 16) and 1 ml of triethylamine. The resultant reaction solution was concentrated under reduced pressure, and the residue was dissolved in chloroform and then washed with water. The thus water-washed chloroform layer was dried over anhydrous sodium sulfate, and then purified through a silica gel column chromatograph (chloroform:methanol=98:2 to 96:4 in volume ratio) in odrer to obtain 0.75 g (yield 55%) of 1,3-dimethyl-6-(2-[N-hydroxyethyl-N-[3-(2-phenyl-3-methyl-4-oxo-4H-1-benzopyran-5-yl)oxypropyl]amino]ethyl-amino)-2,4(1H,3H)-pyrimidinedione (the non-oxalate of Compound 17).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05114941 |
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| Source dataset | uspto-grants-1992_05 |
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| ORD ID | ord-69811d6cb42e4ffeb56690794899799e |
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| Source note | uspto-grants-1992_05 |
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