HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 24821335, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 69443896 | HCID 69443896 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 24821335 | HCID 24821335 | 76% |
Reaction Steps
To a solution of Example 1F (0.15 g, 0.0004 mol) and excess triethylamine (2 mL) in methylene chloride (5 mL) was added excess acetic anhydride (1 mL) and the mixture was stirred at room temperature for 15 minutes. After quenching with methanol (5 mL), the solvent was concentrated and the residue was purified on silica gel (50˜75% ethyl acetate in hexane) to give 0.12 g of the title compound (76% yield). 1H NMR (300 MHz, CDCl3) δ ppm 1.35 (d, J=6.25 Hz, 6 H) 1.49 (d, J=6.99 Hz, 3 H) 2.00 (s, 3 H) 4.44-4.60 (m, 1 H) 5.06-5.20 (m, 1 H) 5.67 (d, J=6.99 Hz, 1 H) 6.87-6.97 (m, 2 H) 7.16-7.24 (m, 2 H) 7.27-7.34 (m, 2 H) 7.37 (s, 1 H) 7.38-7.44 (m, 2 H). MS (ESI), m/z 396.9 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08735595B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-b9bbf0e13efa442c888db017956231b7 |
| Source note | uspto-grants-2014_05 |