HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric acid magnesium salt (1:1) → HCID 178480587, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | 1-Methyl-2-imidazolecarboxaldehyde | HCID 139575 | — |
| Reactant | 4-Amino-6-fluoroisobenzofuran-1(3H)-one | HCID 67258974 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 178480587 | HCID 178480587 | 68.7% |
Reaction Steps
A solution of 1-methyl-1H-imidazole-2-carbaldehyde (659 mg, 6.0 mmol), 4-amino-6-fluoroisobenzofuran-1(3H)-one (1.0 g, 6.0 mmol), and anhydrous magnesium sulfate (7.2 g, 60.0 mmol) in acetonitrile (100 mL) was heated to reflux for 2 days. The solution was filtered and the solvents were removed in vacuum. The crude product was re-crystallized from isopropanol to afford the title compound (1.068 g, yield 68%) LC-MS (ESI) m/z: 260 (M+1)+. 1H-NMR (400 MHz, DMSO-d6) δ (ppm): 4.04 (s, 3H), 5.49 (s, 2H), 7.24 (s, 1H), 7.54-7.58 (m, 2H), 7.73-7.76 (m, 1H), 8.70 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08012976B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-d3a880b95d054df281bccba125647fa0 |
| Source note | uspto-grants-2011_09 |