HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 135890157, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 2,5-Hexanedione | HCID 8035 | — |
| Reactant | HCID 136197415 | HCID 136197415 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 135890157 | HCID 135890157 | 44% |
Reaction Steps
The compound (200 mg, 0.66 mmol) of example 42 and 2,5-hexanedione (76 mg, 0.66 mmol) were dissolved in ethanol (10 ml) and added with glacial acetic acid (0.1 ml), followed by refluxing for 12 h. The reaction mixture was concentrated to dryness, dissolved in CH2Cl2 (10 ml), and washed with saturated NaHCO3 (10 ml) and saturated saline (10 ml), dried and concentrated. The residue was passed through a silica gel column to give the title compound (110 mg, yield: 44%). 1H NMR (CDCl3) δ: 11.20 (1H, br), 8.42 (1H, d), 7.30 (1H, dd), 7.10 (1H, d), 5.93 (2H, s), 4.23 (2H, t), 2.63 (2H, q), 2.59 (2H, q), 2.06 (6H, s), 2.04 (2H, m), 1.24 (3H, t), 1.18 (3H, t), 1.15 (3H, t).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08871777B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-f4864c18f916415bab595628d0c51150 |
| Source note | uspto-grants-2014_10 |