Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Putrescine | HCID 1045 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 4-Chloro-3-nitropyridine | HCID 2735781 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 19864520 | HCID 19864520 | — |
Reaction Steps
To a solution of 1,4-diaminobutane (8.8 g) in ethanol (100 ml) at room temperature was added a solution of 4-chloro-3-nitropyridine in ethanol (50 ml). The mixture was stirred at room temperature for 30 minutes, poured into ethyl acetate (400 ml), and then washed with water (3×150 ml). The aqueous phases were back-extracted with methylene chloride (3×120 ml) and all the organic phases were combined, dried over Na2SO4, filtered and evaporated under vacuum. The residue was chromatographed on silica eluting with a mixture of methylene chloride and methanol containing 1% ammonium hydroxide. The fractions containing the product were combined and evaporated under vacuum to give the title compound, (4.2 g), which was used directly in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04904671 |
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| Source dataset | uspto-grants-1990_02 |
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| ORD ID | ord-2edd9f1a6cf84295bd76af664d581272 |
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| Source note | uspto-grants-1990_02 |
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