HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formamidine acetate → HCID 178494687, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formamidine acetate | HCID 160693 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | Methyl 4-methoxy-2-methylacetoacetate | HCID 11084163 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178494687 | HCID 178494687 | 61.4% |
Reaction Steps
To a solution of methyl 2-methyl-4-(methyloxy)-3-oxobutanoate (Intermediate 47, 1.01 g, 6.31 mmol) in methanol (7 mL) was added formamidine acetate (0.722 g, 6.94 mmol) and 25% sodium methoxide in MeOH (3.0 mL, 6.31 mmol) and the resulting mixture was heated under reflux for 2 hours, cooled to room temperature and left to stand overnight. The reaction mixture was evaporated under reduced pressure. The residue was diluted with water, adjusted to pH 7 using aqueous 2M HCl solution and extracted with chloroform (×3). The chloroform layers were combined, dried under magnesium sulfate and evaporated under reduced pressure to give the title compound as a white solid (597 mg);
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796283B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-fe69e65e7bb2454d97f964bcd8afab41 |
| Source note | uspto-grants-2014_08 |