HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric acid magnesium salt (1:1) → HCID 178483209, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | 4-Dimethylaminomethylbenzaldehyde | HCID 193251 | — |
| Reactant | 4-Amino-6-fluoroisobenzofuran-1(3H)-one | HCID 67258974 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 178483209 | HCID 178483209 | 60.1% |
Reaction Steps
A solution of 4-((dimethylamino)methyl)benzaldehyde (1.0 g, 6.13 mmol), 4-amino-6-fluoroisobenzofuran-1(3H)-one (1.024 g, 6.13 mmol) and anhydrous magnesium sulfate (7.356 g, 61.3 mmol) in acetonitrile (50 ml) was heated at reflux for 2 days. The solution was filtered and concentrated in vacuum. The crude product was re-crystallized with isopropanol to obtain the title compound (1.15 g, yield 60%). LC-MS (ESI) m/z: 313 (M+1)+. 1H-NMR (400 MHz, CDCl3) δ (ppm): 2.28 (s, 6H), 3.52 (s, 2H), 5.38-5.38 (m, 2H), 7.09-7.12 (m, 1H), 7.42-7.44 (m, 1H), 7.46-7.48 (d, J=8 Hz, 2H), 7.87-7.89 (d, J=8 Hz, 2H), 8.51 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08012976B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-070d7e7f381a4b18bcd399c482575c5e |
| Source note | uspto-grants-2011_09 |