HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl acetoacetate → HCID 86714154, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl acetoacetate | HCID 7757 | — |
| Reactant | Methyl propiolate | HCID 13536 | — |
| Reactant | 4-Aminomethyltetrahydropyran | HCID 2773210 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86714154 | HCID 86714154 | 90.3% |
Reaction Steps
A mixture of 4-aminomethyltetrahydropyran (1.02 g, 8.9 mmol) and 3-oxo-butyric acid methyl ester (1.15 mL, 10.6 mmol) in MeOH (40 mL) was refluxed for 2 h. Propynoic acid methyl ester (1.2 mL, 13.3 mmol) was added, and the resulting mixture was refluxed for 48 h. After cooling to r.t., the solvent was evaporated, and the crude oil was recrystallized from MeOH to give 2.39 g of the title compound as an off-white solid. MS: (+) m/z 298.33 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09271970B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-d4de8756353049f5b9def7f614170256 |
| Source note | uspto-grants-2016_03 |