Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 131721749 | HCID 131721749 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22252177 | HCID 22252177 | 13% |
Reaction Steps
Into a solution of Example 28 (0.2 g, 0.4 mmol) in 50 mL of MeOH was bubbled ammonia and the resulting mixture was stirred at 35° C. for two days. The mixture was concentrated in vacuo to give a residue which was washed with 2×30 mL of water. Extraction, drying over MgSO4 and concentration in vacuo gave a residue that was purified via radial chromatography using DCM:MeOH (90:10) as eluting solvent and via preparative chromatography (20×20- cm plate, 0.5 mm, SiO2) using the same eluant. The title compound (0.025 g, 13%) was isolated as white crystals after recrystallization from MeOH:H2O. MP: 183° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06043252 |
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| Source dataset | uspto-grants-2000_03 |
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| ORD ID | ord-135b843f79f847f487174997ba18253c |
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| Source note | uspto-grants-2000_03 |
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