HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl methyl ether → HCID 86634374, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl methyl ether | HCID 15413 | — |
| Reactant | 1-(2-Chloropyrimidin-4-yl)azepane | HCID 15175748 | — |
| Reactant | HCID 86634373 | HCID 86634373 | — |
| Solvent | Cyclohexanol | HCID 7966 | — |
| Product | HCID 86634374 | HCID 86634374 | 46% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
To a solution of the compound 7 (240 mg) in cyclohexanol (0.4 mL), 1-(2-chloro-4-pyrimidinyl)azepane (210 mg) was added. The reaction mixture was stirred at 120° C. for 3.5 hours. After cooling to room temperature, the reaction mixture was added tert-butyl methyl ether, washed with aqueous 2N sodium hydroxide solution, dried over anhydrous magnesium sulfate and then concentrated. The obtained residue was purified by silica gel column chromatography (ethyl acetate:methanol:27% aqueous ammonia=100:0:0→90:10:0→90:10:1) to obtain the title compound (190 mg) having the following physical properties.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680092B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-ad2ff19fed9d453387f676f18eab6127 |
| Source note | uspto-grants-2014_03 |