HuagongsheHuagongshe Chemistry Print Report · For research reference only
Propanedioic acid, monoethyl ester → HCID 136344290, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Propanedioic acid, monoethyl ester | HCID 3595298 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 178426522 | HCID 178426522 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 136344290 | HCID 136344290 | 90% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
1.2 g of sodium are added in a fractionated way to 15 mL of MeOH. After total dissolution, 3 g of 4,4-dimethyl-1,4,5,6-tetrahydropyrimidin-2-amine solubilized beforehand in 5 mL of MeOH are added, and then 14.4 mL of ethyl malonate. 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 conc.HCl down to pH 3-4. The formed precipitate is filtered, washed with ether and dried in the oven in vacuo. 1.14 g (yield=90%) of 2-hydroxy-8,8-dimethyl-6,7,8,9-tetrahydro-4H-pyrimido[1,2-a]pyrimidin-4-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-dfb5d59ee9944e2fac27abefb7829eeb |
| Source note | uspto-grants-2014_08 |