Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Sulfate → 3-{3-[(3-Methylpiperidin-1-yl)methyl]phenoxy}propan-1-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Sulfate | HCID 24436 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 3-[(3-Methylpiperidin-1-yl)methyl]phenol | HCID 13364666 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-{3-[(3-Methylpiperidin-1-yl)methyl]phenoxy}propan-1-amine | HCID 14026188 | — |
반응 단계
5.13 g (0.025 mol) of 3-[(3-Methylpiperidin-1-yl) methyl]phenol are introduced into a suspension of 1.0 g (0.025 mol) of sodium hydride (60%) in absolute DMF and stirred overnight at room temperature. After the addition of 2.23 g (0.025 mol) of 3-chloropropionic acid nitrile, the reaction mixture is stirred for 7 hours at 60° C. and then poured into ice water and extracted with ether, and the organic phase is washed with 5% NaOH. After dehydration over Na2SO4, the ethereal phase is introduced dropwise into a suspension of 1.14 g (0.03 mol) of LiAlH4 in absolute ether and then hydrolysed with 2.2 ml of H2O. After filtration and removal of solvent by evaporation under vacuum, 2.96 g of a pale yellow oil are left behind.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04727081 |
| 출처 데이터셋 | uspto-grants-1988_02 |
| ORD ID | ord-055eb18c1384484c97946551c03e5d3e |
| 출처 메모 | uspto-grants-1988_02 |