HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 18425486, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 12991339 | HCID 12991339 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Water ethylacetate | HCID 22728543 | — |
| Product | HCID 18425486 | HCID 18425486 | 81% |
Reaction Steps
A mixture of 7-benzylthio-3-(2-chlorophenyl)-1-(ethoxycarbonylmethyl)-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one (1.435 g, 3.36 mmol) and lithium hydroxide monohydrate (481 mg, 11.5 mmol) in methanol (10 mL) and water (30 mL) were refluxed for 48 hours. The reaction mixture was cooled to room temperature and diluted with ethyl acetate/water. The aqueous layer was adjusted to pH 4 and extracted with ethyl acetate. The combined organic extracts were dried, filtered and concentrated in vacuo to give 1.2 g of 7-benzylthio-3-(2-chlorophenyl)-1-(hydroxycarbonylmethyl)-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06451804B1 |
| Source dataset | uspto-grants-2002_09 |
| ORD ID | ord-b162ff67349a4cc1918721e83408176e |
| Source note | uspto-grants-2002_09 |