Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 385194 | HCID 385194 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 385198 | HCID 385198 | 72.4% |
Reaction Steps
To 2-amino-4-[[(1-hydroxymethyl-1-cyclobutyl)methyl]amino]pyrimidine (0.21 g, 1.0 mmol) was added acetic acid (3 ml) and the mixture was heated to 110° C. Sodium acetate 3 hydrate (0.18 g) was added and bromine (60 μl) dissolved in acetic acid (0.5 ml) was dropwise added at 70° C. After cooling, water was added to the reaction mixture and the mixture was neutralized with aqueous ammonia under ice-cooling, extracted with ethyl acetate and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was recrystallized from acetone to give colorless prism crystals (0.21 g, 72.4%), m.p. 156-158° C. (acetone).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06080750 |
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| Source dataset | uspto-grants-2000_06 |
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| ORD ID | ord-e789c5d0393a40449349d26c8ae6d3d4 |
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| Source note | uspto-grants-2000_06 |
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