HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Bromohexane → HCID 178444682, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Bromohexane | HCID 8101 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 178421604 | HCID 178421604 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Ammonia | HCID 222 | — |
| Product | HCID 178444682 | HCID 178444682 | 18.6% |
Reaction Steps
To a solution of 4-methyl-4-(3-(1H-1,2,4-triazol-3-yl)phenyl)piperidine (Preparation 45, 55 mg, 0.23 mmol) in N,N-dimethylformamide (2 mL) was added sodium hydrogencarbonate (28 mg, 0.34 mmol) and bromohexane (32 μL, 0.23 mmol). The resultant mixture was heated at 50° C. for 2 h and then allowed to cool. The mixture was partitioned between water (5 mL) and dichloromethane (20 mL). The layers were separated, and the aqueous layer was extracted with dichloromethane (20 mL). The combined extracts were dried over Na2SO4, filtered and concentrated in vacuo and the residue was purified by silica (5 g) column chromatography eluting with methanol:dichloromethane:0.88 ammonia (10:90:1) to give the title compound as a clear oil (7 mg, 9%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06750231B2 |
| Source dataset | uspto-grants-2004_06 |
| ORD ID | ord-d9dc504467124fc1881a73347d452b45 |
| Source note | uspto-grants-2004_06 |