HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 60171307, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-(4-Chlorophenyl) glutarate | HCID 607276 | — |
| Product | HCID 60171307 | HCID 60171307 | 70.7% |
Reaction Steps
A solution of 3-(4-chlorophenyl)glutaric acid (1.0 g, 4.1 mmol) in acetic anhydride (20 mL, 200 mmol) was heated to reflux, stirred for 17 h, cooled at room temperature, and concentrated to dryness. The crude residue was dried under vacuum for 1 h. The crude anhydride was dissolved in ethanol (30 mL) and triethylamine (3.0 mL, 22 mmol) was added. The reaction was stirred for 17 h at room temperature and then concentrated to dryness. The crude residue was dissolved in dichloromethane (5 mL) and purified on SiO2 (40 g) using 5% MeOH/DCM to provide the title product (0.785 g, 70% yield) as a clear oil. 1H NMR (DMSO-d6, 400 mHz) δ (ppm): 12.09 (s, 1H), 7.30-7.22 (m, 4H), 3.93-3.87 (m, 2H), 3.4 (m, 1H), 2.71-2.46 (s, 4H), 1.0 (t, J=7 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08497287B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-e976053cea114fbe8b8b5c7512480a2e |
| Source note | uspto-grants-2013_07 |