HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 54390795, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-chloro-N-methylacetamide | HCID 66773 | — |
| Reactant | Bis(4-fluorophenyl)(piperidin-4-yl)methanol | HCID 11208889 | — |
| Catalyst | Potassium Iodide | HCID 4875 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 54390795 | HCID 54390795 | 95% |
Reaction Steps
A mixture of 12.1 g (0.040 mole) of α,α-bis(4-fluorophenyl)-4-piperidinemethanol, 5.2 g (0.048 mole) of 2-chloro-N-methylacetamide, 17.0 g (0.160 mole) of anhydrous sodium carbonate and 0.4 g (0.002 mole) of potassium iodide in 100 mL of N,N-dimethylformamide was heated on a steam bath for 16 h. The mixture was poured into 1.5 L of water and extracted twice with 500 mL portions of ethyl acetate. The ethyl acetate layers were combined, washed with water and brine, dried (MgSO4), and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate to yield 14.2 g (95%) of white solid, mp 122°-124° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05057524 |
| Source dataset | uspto-grants-1991_10 |
| ORD ID | ord-a8a4b5f64ad94e938c1e071782d66b0a |
| Source note | uspto-grants-1991_10 |