Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 57437662 | HCID 57437662 | — |
| Solvent | Trifluoroacetic anhydride | HCID 9845 | — |
| Product | HCID 57437664 | HCID 57437664 | — |
Reaction Steps
Compound 6 (6.82 grams, 34.5 mmol) was added in portions to trifluoroacetic anhydride (50 mL) cooled to 0° C. After 15 minutes the sodium chloride ice water bath was replaced with a dry ice acetone bath and nitric acid (6.0 mL 70%) was added drop wise. This was stirred to ambient temperature for 16 hours after which time it was pored into ice-water and neutralized with solid sodium bicarbonate. The product was extracted with dichloromethane and purified on a silica gel flash column eluted with 49:1 dichloromethane-methanol to give the desired product as an orange paste. LCMS data supported the structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08889864B2 |
|---|
| Source dataset | uspto-grants-2014_11 |
|---|
| ORD ID | ord-0d04ce1a50724a17beb238f27b651dba |
|---|
| Source note | uspto-grants-2014_11 |
|---|