HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 57467473, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | HCID 57467472 | HCID 57467472 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57467473 | HCID 57467473 | — |
Reaction Steps
To a solution of Example 53C (8 g, 34.5 mmol) in dichloromethane (100 mL) and triethylamine (19.25 mL, 138 mmol) was added trifluoroacetic anhydride (slow addition, 14.63 mL, 104 mmol) at 0° C. After the addition, the solution was allowed to warm to room temperature and stirred for 2 hours before methanol (20 mL) was added to quench the reaction. The solution was washed with saturated NaHCO3 solution, dried (Na2SO4), and concentrated. The residue was purified by column chromatography using an Analogix® Intelliflash280™ (SiO2, 0-60% ethyl acetate in hexanes) to provide titled product. MS (DCI+) m/z 214 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08507493B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-c6327ce61f9f429e84cc46a484d833a7 |
| Source note | uspto-grants-2013_08 |