反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Under nitrogen atmosphere, at 0° C., to a stirring mixture of LiAlH4 (0.46 g, 12.23 mmol) in dry Et2O (5 mL), 5-(4-fluorophenyl)-pentanoic acid (0.6 g, 3.05 mmol) in dry Et2O (35 mL) was added dropwise. The mixture was left to react at rt for 4 h, then at 0° C. H2O (0.46 mL), 3M KOH solution (0.46 mL) and H2O (1.54 mL) were very slowly added. The mixture was stirred for 1 h at 0° C., filtered to remove the solid residue, and the organic phase dried over Na2SO4. The organic solution was again filtered and concentrated to dryness affording the title compound (0.53 g, 95%) as a colorless oil. 1H NMR (CDCl3): δ 1.36-1.47 (m, 2H), 1.58-1.71 (m, 4H), 2.58-2.65 (m, 2H), 3.66 (t, J=5.8 Hz, 2H), 6.94-7.02 (m, 2H), 7.11-7.17 (m, 2H).
WORKUP
后处理
- additionwas added dropwise
- waitThe mixture was left
- customto react at rt for 4 h
- customat 0° C
- filtrationfiltered
- customto remove the solid residue
- dry with materialthe organic phase dried over Na2SO4
- filtrationThe organic solution was again filtered
- concentrationconcentrated to dryness