HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 10342570, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 6-Chloro-3-(piperidin-4-yl)benzo[d]isoxazole | HCID 13076430 | — |
| Reactant | 1-[4-(2-Chloroethoxy)-3-methoxyphenyl]ethanone | HCID 14407170 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 10342570 | HCID 10342570 | 98.2% |
Reaction Steps
A stirred mixture of 6-chloro-3-(4-piperidinyl)-1,2 benzisoxazole (4.6 g, 19 mmol), 1-[4-(2-chloroethoxy)-3- methoxyphenyl]ethanone (4.3 g, 19 mmol), K2CO3 (2.8 g), a few crystals of KI and acetonitrile (120 ml) was refluxed for 16 hours. The reaction was filtered and the filtrate was concentrated to yield 8.0 g of yellow solid. The solid was chromatographed on a Waters Prep 500 LC (silica columns, eluting with methylene chloride/methanol, 5%). Concentration of the appropriate fractions yielded 3.2 g of a light yellow solid, which upon recrystallization from ethyl acetate afforded 2.3 g (28%) of 1-[4-[2-[4-(6-chloro-1,2-benzisoxazol-3-yl)-1-piperidinyl]-3-methoxyphenyl]ethanone as a pale yellow solid, m.p. =133°-135° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05612342 |
| Source dataset | uspto-grants-1997_03 |
| ORD ID | ord-8305fb68d0084331817054e48ae7998a |
| Source note | uspto-grants-1997_03 |