Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Calciumoxide | HCID 6850728 | — |
| Reactant | N-(3-aminopropyl)pyrimidin-2-amine | HCID 14397405 | — |
| Reactant | HCID 18980288 | HCID 18980288 | — |
| Product | HCID 18980280 | HCID 18980280 | 36% |
Reaction Steps
A mixture of 5-(3-chloropropoxy)-2,3-dihydro-1,4-benzodioxin (0.017 mol), N-2-pyrimidinyl-1,3-propanediamine (0.026 mol) and calcium oxide (5 g) in tetrahydrofuran (150 ml) was stirred overnight at 160° C. (pressure vessel). The mixture was cooled, filtered and the filtrate was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /(CH3OH/NH3)95/5). The pure fractions were collected and the solvent was evaporated, yielding 2.66 g N-[3-[(2,3-dihydro-1,4-benzodioxin-5-yl)oxy]propyl]-N'-2-pyrimidinyl-1,3-propanediamine ethanedioate(1:1) (36.0%); mp. 200.2° C. (comp. 8)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05677310 |
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| Source dataset | uspto-grants-1997_10 |
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| ORD ID | ord-03568a1a619c4f01a2fb82f31c841667 |
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| Source note | uspto-grants-1997_10 |
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