HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 57467467, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | HCID 57467466 | HCID 57467466 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57467467 | HCID 57467467 | — |
Reaction Steps
To a solution of Example 51A (0.9 g, 4.0 mmol) in methylene chloride (10 mL) and triethylamine (2.2 mL, 15.8 mmol) was added 2,2,2-trifluoroacetic anhydride (1.6 mL, 11.9 mmol) at 0° C. The reaction mixture was allowed to warm to room temperature and stirred for three hours before methanol was added to quench the reaction. The reaction mixture was washed with saturated aqueous NaHCO3 solution, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography using an Analogix® Intelliflash280™ (SiO2, 0-100% methanol/ethyl acetate(1/10) in hexanes) to obtain the titled compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.71 (s, 6H), 7.08-7.18 (m, 1H), 7.36-7.49 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08507493B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-44c437e655ad4dc0b5c70ea3c452657a |
| Source note | uspto-grants-2013_08 |