HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 59603146, compound → HCID 59603182, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 59603146 | HCID 59603146 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 59603182 | HCID 59603182 | 28% |
Reaction Steps
A stirred solution of 39 (1.2 g, 4.0 mmol) in acetic acid (35 mL) was refluxed for 16 h. After cooling, the solution was evaporated to dryness. The crude product was adsorbed on silica gel and purified by flash chromatography, eluting with hexane/EtOAc (2:1) to give 40 (230 mg, 28%) as a white solid. 1H NMR (500 MHz, CDCl3): δ: 9.89 (1H, s, CHO), 7.50 (1H, s, H-3), 6.69 (1H, d, J4,6=2.2 Hz, H-6), 6.64 (1H, d, J4,6=2.2 Hz, H-4), 4.01 (3H, s, OMe), 3.87 (3H, s, OMe). 13C NMR CDEPT 135, (500 MHz, CDCl3): δ: 179.91 (CHO), 153.37 (C-2), 116.10 (C-3), 101.80 (C-6), 94.90 (C-4), 56.20 (OMe), 55.88 (OMe).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08283340B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-09f3453b49a34e24a5a2f1eb97ef929e |
| Source note | uspto-grants-2012_10 |