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
- 25 °C
PROCEDURE
实验过程
To a solution of 3-{4-[5-(tert-butyl-dimethyl-silanyloxymethyl)-4-methoxy-thiophen-2-ylmethoxy]-2-fluoro-phenyl}-propionicacid ethyl ester (0.5 g, 1.0 mmol) in THF (5 mL) is added tetra-n-butylammoniumfluoride (1M solution in THF, 2 mL, 2.0 mmol) at 0° C. and the reaction mixture is stirred for 30 minutes at 25° C. The reaction mixture is quenched with water and evaporated to a residue. The residue is extracted with EtOAc, washed with water (15 mL) and brine (15 mL), dried over sodium sulfate, filtered, and concentrated to give the title compound (0.4 g,). 1H NMR (400 MHz, DMSO d6) δ7.41 (s, 1H), 7.19-7.15 (t, J=8.8 Hz, 1H), 6.85-6.75 (m, 2H), 5.32 (br, 1H), 4.85 (s, 2H), 4.55 (s, 2H), 4.04-4.00 (q, J=7.2 Hz, 2H), 3.75 (s, 3H), 3.58 (s, 1H) 3.16-3.12 (t, J=15.2 Hz, 3H), 2.79-2.76 (t, J=14.8 Hz, 2H), 2.55-2.51 (t, J=15.2 Hz, 2H), 1.28-1.22 (t, J=7.2 Hz, 3H),
WORKUP
后处理
- customThe reaction mixture is quenched with water
- customevaporated to a residue
- extractionThe residue is extracted with EtOAc
- washwashed with water (15 mL) and brine (15 mL)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated