HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl chloroformate → HCID 11503063, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 11494661 | HCID 11494661 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11503063 | HCID 11503063 | 42% |
Reaction Steps
Methyl chloroformate (0.13 g, 1.38 mmol) was added to a solution of 2-((2S)-2-(4-aminophenyl)morpholine-4-yl)-6-(3-fluoropyridin-4-yl)-3-methyl-3H-pyrimidin-4-one obtained in Example 13 (0.35 g, 0.92 mmol) and triethylamine (0.25 g, 2.47 mmol) in tetrahydrofuran (20 ml) and the solution was stirred at room temperature for one hour. The mixture was partitioned between water and chloroform. The organic layer was washed with brine, dried over magnesium sulfate, and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting 5-10% methanol in chloroform to furnish methyl (4-((2S)-4-(6-(3-fluoropyridin-4-yl)-3-methyl-4-oxo-3H-pyrimidin-2-yl)morpholin-2-yl)phenyl)carbamate (0.17 g, 42%) as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08129377B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-760f2986686d42e2b3b261012bd44815 |
| Source note | uspto-grants-2012_03 |