Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 9814184 | HCID 9814184 | — |
| Solvent | Formic Acid | HCID 284 | — |
| Product | HCID 86590302 | HCID 86590302 | 49% |
Reaction Steps
A mixture of 5 mL of acetic anhydride and 1.8 mL of 96% formic acid was heated to 70° C. for 3 hours. The solution was allowed to cool whereupon the obtained amine from Example 263 (32 mg, 0.12 mmol) was added. The mixture was stirred for 4 days and then poured into 50 mL of dilute HCl. The mixture was extracted with ethyl acetate, the combined extracts were washed with saturated sodium carbonate and then water, dried (MgSO4), and evaporated. Purification of the resulting product by preparative HPLC using a gradient of 30%-70% acetonitrile/water +0.1% TFA over 40 minutes afforded 18 mg (49%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06232320B1 |
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| Source dataset | uspto-grants-2001_05 |
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| ORD ID | ord-c1ddff6dbd0d4f3dbcb1958f16fff465 |
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| Source note | uspto-grants-2001_05 |
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