Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Decanoyl chloride → 3-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propyl decanoate fumarate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Decanoyl chloride | HCID 66982 | — |
| 반응물 | Fumaric Acid | HCID 444972 | — |
| 반응물 | 3-(4-(6-Fluorobenzo[d]isoxazol-3-yl)piperidin-1-yl)propan-1-ol | HCID 15384966 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propyl decanoate fumarate | HCID 21960039 | — |
반응 단계
To a solution 3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propanol (1.81 g, 6.5 mmol) triethylamine (0.9 g, 9.0 mmol) in DCM (45 ml) was added decanoyl chloride (1.5 g, 7.8 mmol) dropwise at room temperature. The mixture was stirred for 20 minutes, then concentrated down to a crude solid. The solid was extracted into EtOAc (20 ml), and the insoluble salts were filtered. The EtOAc was removed. The crude oil was purified by flash choursomatography (Sorbsil C-30, 30 g; eluted with MeOH:DCM). The oil thus obtained (2.54 g, 90%) was converted to a fumarate salt with fumaric acid (670 mg) in ethanol. The crystals collected weighed 1.61 g, m.p.=100°-102° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05624927 |
| 출처 데이터셋 | uspto-grants-1997_04 |
| ORD ID | ord-7026940dfaf0491ea9894592353f2ecd |
| 출처 메모 | uspto-grants-1997_04 |