Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → Tert-butyl 4-((2-(2,4-dimethoxybenzylamino)pyridin-3-yl)methylamino)piperidine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
| 반응물 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 반응물 | 3-(Aminomethyl)-N-(2,4-dimethoxybenzyl)pyridin-2-amine | HCID 22293160 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Sodium Carbonate | HCID 10340 | — |
| 생성물 | Tert-butyl 4-((2-(2,4-dimethoxybenzylamino)pyridin-3-yl)methylamino)piperidine-1-carboxylate | HCID 22293293 | 69% |
반응 단계
To a stirred solution of N-(2,4-Dimethoxybenzyl)-3-(aminomethyl)pyridin-2-amine (2.04 mmol) and tert-butyl 4-oxopiperidine-1-carboxylate (0.41 g, 2.04 mmol) in DCE (8 ml) and AcOH (115 μL, 2.04 mmol) was added NaBH(OAc)3 (0.43 g, 2.04 mmol) and the reaction stirred at RT until judged complete by LCMS. The reaction mixture was diluted with DCM and sat. aq. Na2CO3, the layers were separated and the organic layer was dried (Na2SO3) and evaporated to dryness. Purification by column chromatography (MeOH/DCM) gave the desired product (0.64 g, 69%). LC/MS (10% to 99%): M/Z (M+H)+ (obs)=457; tR=2.19.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07834000B2 |
| 출처 데이터셋 | uspto-grants-2010_11 |
| ORD ID | ord-32427160f2b647bca3fba4e710178cec |
| 출처 메모 | uspto-grants-2010_11 |