HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Bromopropane → (3R,5R,6S)-3-allyl-5-(3-chlorophenyl)-6-(4-chlorophenyl)-1-propylpiperidin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Bromopropane | HCID 7840 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | (3R,5R,6S)-3-allyl-5-(3-chlorophenyl)-6-(4-chlorophenyl)piperidin-2-one | HCID 58573283 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | (3R,5R,6S)-3-allyl-5-(3-chlorophenyl)-6-(4-chlorophenyl)-1-propylpiperidin-2-one | HCID 67998583 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a solution of (3R,5R,6S)-3-allyl-5-(3-chlorophenyl)-6-(4-chlorophenyl)piperidin-2-one (Example 42, Step A) (70 mg, 0.19 mmol) in 430 μL of DMF was added sodium hydride (60% suspension in mineral oil, 20 mg, 0.51 mmol) at 0° C. The reaction was stirred at 0° C. for 15 min and then treated with 1-bromopropane (53 μL, 0.58 mmol). After being stirred at 25° C. for 4 h, the reaction was quenched with sat. aqueous NaHCO3 and extracted (2×EtOAc). The combined organic layers were washed with sat. aq. NaCl and NaHCO3-solutions, dried over Na2SO4, filtered and the filtrate was concentrated under reduced pressure. Purification of the residue by silica gel prep plate (25% EtOAc/hexanes) provided the title compound as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09296736B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-4a2fb302f9984b6d9383044e9b8a427e |
| Source note | uspto-grants-2016_03 |