Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | Phenyl glycidyl ether | HCID 31217 | — |
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 20237821 | HCID 20237821 | — |
| Reactant | HCID 20237851 | HCID 20237851 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethanol ethylacetate | HCID 21584252 | — |
| Product | HCID 178521322 | HCID 178521322 | — |
Reaction Steps
1.22 g. phenyl glycidyl ether and 3.7 g. 1-(2-aminoethylamino)-pyrimido[4,5-d]indole (prepared by reacting 1-chloropyrimido[4,5-b]indole with an excess of ethylenediamine) are stirred for 7 hours at 50° C., in 20 ml. dimethylformamide. The reaction mixture is then evaporated and the residue is purified chromatographically over a silica gel column using, as elution agent, methylene chloride-methanol-triethylamine (10:2:0.3 v/v/v). The residue obtained by evaporation of the pure fractions is mixed in ethyl acetate-ethanol with fumaric acid and the product obtained is recrystallized from ethanol. There is obtained 0.3 g. (15% of theory) of colorless crystals: m.p. 187°-188° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04438128 |
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| Source dataset | uspto-grants-1984_03 |
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| ORD ID | ord-03459c257805455fa50b860dea150893 |
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| Source note | uspto-grants-1984_03 |
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