HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 20068665, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 20068643 | HCID 20068643 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 20068665 | HCID 20068665 | 23.9% |
Reaction Steps
1-[3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl]-4-(5-fluoro-2-methylthio-2-pyrimidinyl)piperazine hydrochloride (7.45 g, 0.0.17 mole), triethylamine (3.05 g, 0.034 mole) and 2 teaspoons of Raney Nickel in water were mixed in EtOH (125 mL) and refluxed 18 h. The hot reaction mixture was filtered and the filtrate was concentrated in vacuo to about 1/5 volume. A crude crystalline product was obtained by filtration and its recrystallization from 20-25 mL EtOH gave 1.6 g of solid, m.p. 220°-222° C. This solid was converted to the hydrochloride salt in EtOH using ethanolic HCl. Filtration and drying gave 1.6 g of product, m.p. 242°-244° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04994460 |
| Source dataset | uspto-grants-1991_02 |
| ORD ID | ord-5f9e8c277af945feac9aab8ee44f73fe |
| Source note | uspto-grants-1991_02 |