참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | 4-tert-Butylbenzylamine | HCID 2735655 | — |
| 반응물 | Sodium cyanoborohydride | HCID 5003444 | — |
| 반응물 | 2-Chloro-4-ethynylpyridine | HCID 23436831 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Sodium Hydroxide | HCID 14798 | — |
| 생성물 | (4-Tert-butyl-benzyl)-[2-(2-chloro-pyridin-4-yl)-ethyl]-amine | HCID 86613990 | 55.4% |
반응 단계
A mixture of 1.386 g of 2-chloro-4-ethynyl-pyridine (10.07 mmol), 2.65 ml of 4-tert-butyl-benzylamine (15.11 mmol), 0.58 ml of acetic acid (10.07 mmol) and 666 mg of sodium cyanoborohydride (95% purity, 10.07 mmol) in ethanol (12 ml) were heated to 105° C. in a sealed tube for 2 d. The reaction mixture was allowed to cool to RT, diluted with 3N NaOH solution and extracted with DCM. The combined organic extracts were washed with saturated NaHCO3 solution and brine, dried (Na2SO4), filtered and concentrated in vacuo. After column chromatography (heptane/EtOAc 100:0 to 0:100) 1.688 g (55%) of the title compound were isolated as a brown liquid. MS (ISP) 303.2 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07745477B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_06 |
|---|
| ORD ID | ord-ebe208f56ec54742a4158767aa63b045 |
|---|
| 출처 메모 | uspto-grants-2010_06 |
|---|
