HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178525990, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 178501825 | HCID 178501825 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178525990 | HCID 178525990 | 84.3% |
Reaction Steps
A solution of methyl 4-(1,3-dibenzyl-1,2,3,4-tetrahydro-2,4-dioxopyrimidin-5-yl)-2-hydroxy-4-oxobut-2-enoate (3a) (757 mg, 1.8 mmol) in dioxane (100 ml) was refluxed with 1N HCl (60 ml) for 4 h. The solution was evaporated to dryness. The resulting solid vas recrystallized from hexane and ethyl acetate (3:1) to give 617 mg a pale yellow solid. Yield as 84.2%. Mp. 186-188° C. 1HNMR (DMSO-d6): 8.89 (s, 1H), 7.57 (s, 1H), 7.24-7.36 (m, 10H), 5.16 (s, 2H), 5.02 (s, 2H). 13CNMR (DMSO-d6): 186.1, 169.0, 163.2, 159.9, 151.1, 150.2, 136.5, 135.8, 128.7, 128.4, 128.0, 127.8, 127.6, 127.3, 107.7, 100.9, 52.8, 44.2. FAB-HRMS: [M+H]+ Calcd. for C22H19N2O6 407.1243. Found 407.1248.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07569573B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-4afa3aebfaf54e5abc288f681a06f970 |
| Source note | uspto-grants-2009_08 |