HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1-Carbomethoxy-4-[4,4-bis(p-fluorophenyl)butyl]-piperazine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,1'-(4-Chlorobutylidene)bis(4-fluorobenzene) | HCID 76820 | — |
| Reactant | Methyl piperazine-1-carboxylate | HCID 142729 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 1-Carbomethoxy-4-[4,4-bis(p-fluorophenyl)butyl]-piperazine hydrochloride | HCID 20209481 | 17.3% |
Reaction Steps
To a solution of 4.3 g (0.03 mole) 1-carbomethoxypiperazine in 10 ml of ethanol was added 10.0 g (0.036 mole) of 4-chloro-1,1-bis-(p-fluorophenyl)-butane and 5.0 g of sodium bicarbonate. The mixture was heated at reflux for 36 hours. 100 ml of water was added. The mixture was extracted twice with Et2O. The combined extracts were dried over sodium sulphate and concentrated. The residue was dissolved in ethanol-ether and the hydrochloride was precipitated with ethanolic HCl. The solid was collected by filtration and recrystallised from propan-2-ol to give 2.2 g of 1-carbomethoxy-4-[4,4-bis(p-fluorophenyl)butyl]-piperazine hydrochloride. Melting point 192°-193° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04624953 |
| Source dataset | uspto-grants-1986_11 |
| ORD ID | ord-6c0fef2cb14d4383814a1e7140c8c9c5 |
| Source note | uspto-grants-1986_11 |