HuagongsheHuagongshe Chemistry Print Report · For research reference only
Propanedioic acid, monoethyl ester → HCID 136344295, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Propanedioic acid, monoethyl ester | HCID 3595298 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 86700703 | HCID 86700703 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 136344295 | HCID 136344295 | 60% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
1.1 g of sodium are added in a fractionated way to 15 mL of MeOH. After total dissolution, 1.6 g of 5,7-diazaspiro[2.5]oct-5-en-6-amine hydrobromide solubilized beforehand in 5 mL of MeOH, and then 8 mL of ethyl malonate are added. The mixture is heated to 100° C., after 4 h of heating, the medium is dry concentrated. The obtained oil is taken up in ether. The precipitate is filtered and then the residue is taken up in 7 mL of H2O and acidified with concentrated HCl up to pH 3-4. The formed precipitate is filtered, washed with ether and dried in the oven in vacuo. 1.5 g (yield=60%) of 8′-hydroxy-1′,2′-dihydro-spiro[cyclopropane-1,3′-pyrimido[1,2-a]pyrimidin]-6′-one are obtained as a beige solid used as such.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08815853B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-377b78c3c2bd4e5486158cc71eae7103 |
| Source note | uspto-grants-2014_08 |