HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67282022, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Chloro-3-methyl-6-(pyrimidin-4-YL)pyrimidin-4-one | HCID 17954460 | — |
| Reactant | HCID 66718576 | HCID 66718576 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67282022 | HCID 67282022 | 76.7% |
Reaction Steps
To a suspension of optically active 7-(4-bromo-phenyl)-[1,4]oxazepane hydrochloride (0.10 g, 0.34 mmol) and 2-chloro-3-methyl-6-(pyrimidin-4-yl)-3H-pyrimidin-4-one (0.07 g, 0.30 mmol) in tetrahydrofuran (2 mL) was added triethylamine (0.08 mL), 0.60 mmol) at room temperature. The resulting mixture was stirred over night and poured into water. Extractive workup with chloroform was performed and the organic layer was dried over anhydrous sodium sulfate and concentrated. The residue was purified by recrystallization from ethyl acetate and diisopropyl ether to yield (+)-2-[7-(4-bromophenyl)-[1,4]-oxazepane-4-yl]-3-methyl-6-pyrimidin-4-yl-3H-pyrimidin-4-one (A096) (0.10 g, 0.23 mmol, 75%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09108957B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-e4e04121206945ea894131415c5b1c95 |
| Source note | uspto-grants-2015_08 |