HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Iodide → 3-[1-(3-Diethylaminopropyl)-4-piperidyl]-1,2-benzisoxazole difumarate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | 3-Chloropropyl(diethyl)amine | HCID 66918 | — |
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 3-(Piperidin-4-yl)benzo[d]isoxazole | HCID 13076436 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 3-[1-(3-Diethylaminopropyl)-4-piperidyl]-1,2-benzisoxazole difumarate | HCID 13076441 | 28.3% |
Reaction Steps
A suspension of 4.0 g of 3-(4-piperidyl)-1,2-benzisoxazole, 3.2 g of 3-diethylaminopropyl chloride, 3.0 g of potassium iodide and 5.0 g of sodium bicarbonate in 100 ml of butanol was heated under reflux for 2 hrs, cooled to room temperature and filtered. The filitrate was washed with water and extracted with ether (3 times). The ether extracts were dried over anhydrous sodium sulfate, filtered and evaporated to give an oil. The oil was dissolved in 10 ml of acetonitrile and 4.2 g of fumaric acid was added. The mixture was stirred for 2 hrs, filtered and the filter cake was recrystallized three times from ethanol-ether to give 2.8 g (26%) of product, mp 174°-176°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04355037 |
| Source dataset | uspto-grants-1982_10 |
| ORD ID | ord-2f0101fb514c4242b53bbb821d81edc7 |
| Source note | uspto-grants-1982_10 |