HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 5-Methoxycarbonyl-4-(2-ethoxy-6-pentadecylphenyl)-6-methyl-3,4-dihydropyrimidin-2(1H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Urea | HCID 1176 | — |
| Reactant | Methyl acetoacetate | HCID 7757 | — |
| Reactant | 2-Ethoxy-6-pentadecyl benzaldehyde | HCID 22574570 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-Methoxycarbonyl-4-(2-ethoxy-6-pentadecylphenyl)-6-methyl-3,4-dihydropyrimidin-2(1H)-one | HCID 10368710 | — |
Reaction Steps
A solution of methylacetoacetate (1.2 g, 8.5 mmol), 2-ethoxy-6-pentadecyl benzaldehyde (3 g, 8.5 mmol) and urea (1.00 g, 17 mmol) in tetrahydrofuran (20 mL) was heated to reflux (65-70° C.) in the presence of hydrochloric acid (30%) for 7 h. The reaction mixture after being cooled to room temperature was poured into crushed ice (20 g) and stirred for 5 min. The viscous liquid was extracted with ethylacetate (40 mL) and was washed with 1N hydrochloric acid, water, sodium bicarbonate and brine. After drying over anhydrous sodium sulfate, the solvent was evaporated to yield light yellow oil. This crude product was purified by flash column chromatography and recrystallized from hexane to get white crystalline solid of title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08106062B1 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-44a2ff48cc9145b0b73c541a9abdcbbe |
| Source note | uspto-grants-2012_01 |