Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 15751520 | HCID 15751520 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 19101723 | HCID 19101723 | 88.4% |
Reaction Steps
tert-Butyl 4-[2-(benzyloxy)-5-cyclopropyl-8-fluoro-1,2,3,5-tetrahydro-1,3-dioxopyrimido[1,6-a]benzimidazol-7-yl]-1-piperazinecarboxylate (580 mg, 1.05 mmol) is treated with 33 percent hydrobromic acid in glacial acetic acid (5 ml). After 18 hours at room temperature the separated crystals are filtered off, washed with glacial acetic acid and recrystallized from methanol. The crystals are then dissolved in a water/ethanol mixture (2:1, 50 ml). The pH is adjusted to 8 using 1N sodium hydroxide solution, whereby white crystals separate. The crystals are filtered off, washed with water and dried in a high vacuum. There are obtained 417 mg (88%) of 2-(benzyloxy)-5-cyclopropyl-8-fluoro-7-(1-piperazinyl)pyrimido[1,6-a]benzimidazole-1,3(2H,5H)-dione.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05283248 |
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| Source dataset | uspto-grants-1994_02 |
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| ORD ID | ord-b4447a9c46e84aa1926fb730c6ecc93e |
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| Source note | uspto-grants-1994_02 |
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