참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 4-Chlorobutyronitrile | HCID 12336 | — |
| 반응물 | Sodium Sulfate | HCID 24436 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 반응물 | 3-((2-Methylpiperidin-1-yl)methyl)phenol | HCID 53995029 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 4-[3-[(3-Methylpiperidin-1-yl)methyl]phenoxy]butanamine | HCID 14026187 | — |
반응 단계
5.13 g (0.025 mol) of 3-((methylpiperidin-1-yl)methyl) phenol (Example 64 a) are added to a suspension of 1.0 g (0.025 mol) of sodium hydride (60%) in absolute DMF and the mixture is stirred overnight at room temperature. After the addition of 2.58 g (0.025 mol) of 4chlorobutyronitrile, the reaction mixture is stirred at 60° C. for 7 hours, 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 H2O. After removal of the inorganic constituents by filtration and evaporation of the solvent under vacuum, 3.66 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-a74a4d08ee934a7985e29a4219f4899c |
|---|
| 출처 메모 | uspto-grants-1988_02 |
|---|
