HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 10026390, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-(3-Chloropropoxy)-3-methoxyacetophenone | HCID 7314264 | — |
| Reactant | 6-Chloro-3-(piperidin-4-yl)benzo[d]isoxazole | HCID 13076430 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 10026390 | HCID 10026390 | 36.1% |
Reaction Steps
A stirred mixture of 6-chloro-3-(4-piperidinyl)-l,2-benzisoxazole (4.7 g, 20 mmol), 1-[4-(3-chloropropoxy)-3-methoxyphenyl]ethanone (4.8 g, 20 mmol), K2CO3 (2.8 g), several crystals of KI and acetonitrile (120 ml) was refluxed for 16 hours. The reaction was filtered and the filtrate was concentrated to yield a solid-oil mixture. The residue was chromatographed on a Waters Prep 500 utilizing silica columns and eluting with methylene chloride/methanol (5%). Concentration of the desired fractions yielded 3.2 g of a beige solid, which upon recrystallization from ethanol afforded 2.7 g (31%) of 1-[4-[3-[4-(6-chloro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propoxyl-3-methoxyphenyl]-ethanone as a beige solid, m.p.=116°-118° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05629326 |
| Source dataset | uspto-grants-1997_05 |
| ORD ID | ord-a1ddb882fff44a8f957c0f51a34da17c |
| Source note | uspto-grants-1997_05 |