HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl acetoacetate → HCID 135507431, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl acetoacetate | HCID 7757 | — |
| Reactant | 2-(3-Fluorophenyl)ethanamine | HCID 533928 | — |
| Reactant | 26384-76-9 | HCID 135905310 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 135507431 | HCID 135507431 | 10% |
Reaction Steps
Utilizing the methods described in Example 1 the title compound was prepared from 2-hydroxy-benzimidic acid methyl ester (500 mg, 2.67 mmol), 2-(3-fluoro-phenyl)-ethylamine (330 μl, 2.6 mmol) and methyl acetoacetate (3.0 mL) yielding 160 mg (10%) of 3-[2-(3-fluoro-phenyl)-ethyl]-2-(2-hydroxy-phenyl)-6-methyl-3H-pyrimidin-4-one as a white solid after two purifications by flash chromatography on ODS silica gel eluting with methanol-water (4.5:6.5) followed by recrystallization from a large volume of toluene (100 mL).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07491728B2 |
| Source dataset | uspto-grants-2009_02 |
| ORD ID | ord-817c0ca281fb4e07acdadc05e29dd8c5 |
| Source note | uspto-grants-2009_02 |