碘甲烷 → 5-溴-2-(甲氧基甲基)吡啶
反应方程式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][OH:9])=[N:6][CH:7]=1.[H-].[Na+].[CH3:12]I>CN(C=O)C.[Cl-].[Na+].O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][O:9][CH3:12])=[N:6][CH:7]=1参与物
6
实验过程
A solution of this (5-bromo-pyridin-2-yl)-methanol (4.80 g, 23.0 mmol) in DMF (25 mL) was added drop wise over 5 minutes to a slurry of sodium hydride (1.10 g, 27.6 mmol) in DMF (50 mL) at 0° C. under N2. The mixture was stirred for 15 minutes before the drop wise addition of a solution of methyl iodide (1.57 mL, 25.3 mmol) in DMF (25 mL). The mixture was allowed to reach room temperature and was then stirred overnight. The mixture was poured into brine and extracted with EtOAc. The combined organic layers were thoroughly washed with brine, dried over MgSO4 and evaporated to dryness to give the title compound as a yellow oil (4.77 g, 98%) sufficiently pure for the next step.
后处理
- customto reach room temperature
- extractionextracted with EtOAc
- washThe combined organic layers were thoroughly washed with brine
- dry with materialdried over MgSO4
- customevaporated to dryness
来源与证据
- ORD记录
- ord-0943eab2268d4caa99970f06c3ca237a
- 来源数据集
- uspto-grants-2013_12
- 专利号
- US08598213B2
反应笔记
加载中…