Piperidine → 5-Bromo-2-(piperidin-1-yl)pyridine
반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5](OS(C(F)(F)F)(=O)=O)=[N:6][CH:7]=1.[NH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1>CN(C=O)C>[Br:1][C:2]1[CH:7]=[N:6][C:5]([N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)=[CH:4][CH:3]=1참가 물질
4
반응 조건
- 온도
- 40 °C
실험 절차
A mixture of trifluoromethanesulfonic acid 5-bromopyrid-2-yl ester (see step (a) above; 1.5 g, 4.9 mmol), piperidine (1.07 mL, 10.8 mmol) and DMF (5 mL) was heated at 40° C. for 3 h. DMF was then removed in vacuo, water (20 mL) was added to the residue and the product extracted with EtOAc (3×15 mL) and CH2Cl2 (15 mL). The combined organic extracts were washed with brine and dried (Na2SO4). After removal of the solvent, the residue was dissolved in Et2O and HCl (4M in dioxane; 4 mL) was added.
후처리
- customDMF was then removed in vacuo, water (20 mL)
- additionwas added to the residue
- extractionthe product extracted with EtOAc (3×15 mL) and CH2Cl2 (15 mL)
- washThe combined organic extracts were washed with brine
- dry with materialdried (Na2SO4)
- customAfter removal of the solvent
- dissolutionthe residue was dissolved in Et2O
- additionHCl (4M in dioxane; 4 mL) was added
출처 및 근거
- ORD 기록
- ord-5e18a207fb984b58bcb0ac15508d974d
- 출처 데이터셋
- uspto-grants-2010_04
- 특허 번호
- US07705023B2
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