Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 13784089 | HCID 13784089 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 13670001 | HCID 13670001 | 87% |
Reaction Steps
After washing 240 mg of sodium hydride (60% in oil, 6 mmol) with hexane, it was suspended in 3 ml of N,N-dimethylformamide (DMF). Thereafter, a DMF solution (10 ml) of 1.7 g (5 mmol) of 2-(4-benzylpiperazino)-N-ethyl-4-methylpyrimidine-5-carboxylic acid amide (Referential Example 5) was added and the reactants were reacted at 150° C. for 1.5 hours. After distilling off DMF under reduced pressure, 100 ml of water was added, followed by extraction with ethyl acetate. The ethyl acetate layer was washed with saturated saline and dried with magnesium sulfate, and ethyl acetate was distilled off under reduced pressure. The residue was recrystallized from ethyl acetate-hexane to obtain 1.5 g of the intended product as light yellowish crystals (yield: 87%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04734418 |
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| Source dataset | uspto-grants-1988_03 |
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| ORD ID | ord-543e5b35e7a34a518e7484bc0862b37f |
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| Source note | uspto-grants-1988_03 |
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