Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 2304284 | HCID 2304284 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59356612 | HCID 59356612 | 85.4% |
Reaction Steps
Ethyl 2-tert-butyl-6-oxo-1,6-dihydropyrimidine-5-carboxylate (43.9 g) was dissolved in ethanol (200 ml), 2 M aqueous sodium hydroxide solution (330 ml) was added and the mixture was stirred at room temperature for 40 hr. The reaction mixture was concentrated under reduced pressure, and the aqueous layer was adjusted to pH 8 with 6 M hydrochloric acid. The mixture was concentrated under reduced pressure, and subjected to azeotropic distillation with 2-propanol. The residue was suspended in acetone, and insoluble powder was collected by filtration. The obtained powder was suspended in 1 M hydrochloric acid and the suspension was adjusted to pH 3. The suspension was concentrated under reduced pressure. The residue was subjected to azeotropic distillation with 2-propanol, and suspended in acetone. The insoluble material was filtered off and the filtrate was concentrated under reduced pressure to give the object compound (32.8 g) as a powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08329691B2 |
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| Source dataset | uspto-grants-2012_12 |
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| ORD ID | ord-b406494bc394401eaf38a0f4472f84c1 |
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| Source note | uspto-grants-2012_12 |
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