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Potassium Carbonate → N-[2-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl]morpholine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Morpholine, 4-(2-chloroethyl)-, hydrochloride (1:1) | HCID 77210 | — |
| 反応物 | 3-(4-Piperidyl)-6-fluoro-1,2-benzisoxazole | HCID 849421 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[2-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl]morpholine | HCID 21960100 | — |
反応手順
A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.0 g, 13.6 mmol), 2-chloroethyl morpholine hydrochloride (4.46 g, 29.7 mmol) and K2CO3 (7.3 g, 2.2 eq) in acetonitrile (60 ml) was heated at reflux for 24 hours. The crude mixture was diluted with DCM and filtered. The solvent was concentrated to an oil (~7.1 g). Purification on a silica gel column (55 g, SiO2, eluted with MeOH:DCM) yielded a solid product weighing 4 g. Recrystallization from hot ethanol yielded 2.1 g (48%), m.p.=131°-132° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05624927 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-d247b9509078469f8770162921f54760 |
| 出典メモ | uspto-grants-1997_04 |