HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 24821339, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 69189942 | HCID 69189942 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 24821339 | HCID 24821339 | 88% |
Reaction Steps
To a solution of Example 11D ((110 mg, 0.337 mmol) and diisopropylethylamine (0.5 mL) in methylene chloride (1 mL) cooled to 0° C. was added acetic anhydride (100 μL, 1.06 mmol, 3.1 eq.). The mixture was stirred at room temperature overnight. The reaction mixture was purified directly on silica gel eluting with ethyl acetate:hexane gradient (0-80%) to give the title compound (109 mg, 88%). 1H NMR (300 MHz, DMSO-d6) δ ppm 8.30 (d, J=8.09 Hz, 1 H), 7.66 (s, 1 H), 7.45-7.54 (m, 2 H), 7.33-7.40 (m, 2 H), 7.27-7.32 (m, Hz, 2 H), 6.99-7.10 (m, 2 H), 4.77-4.96 (m, 1 H), 3.79 (s, 3 H), 1.83 (s, 3 H), 1.32 (d, J=6.99 Hz, 3 H); MS (DCl) m/e 369 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08735595B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-b477421759f44e95a62d600ff3959660 |
| Source note | uspto-grants-2014_05 |