HRID416979
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
PROCEDURE
实验过程
To a solution of 4-[3-[6-(3-Bromo-5-hydroxymethyl-phenoxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (2.99 g, 5.05 mmol) in DCM (100 mL), TEA (3.52 mL, 25.26 mmol), DMAP (62 mg, 0.505 mmol) were added, followed by MsCl (0.60 mL, 7.58 mmol), and stirred at room temperature for 2.5 h. MeOH (4 mL) was added to quench the reaction. The solvent was removed under reduced pressure. Flash column chromatography (40% EtOAc/Hex) provided a colorless oil (2.51 g, 74% yield). 1H NMR (CDCl3): δ 7.11-7.05 (m, 3H), 6.86 (s, 1H), 6.77 (d, 1H), 6.68 (d, 1H), 5.14 (s, 2H), 4.17-4.08 (m, 4H), 4.01-3.91 (m, 4H), 2.99-2.93 (m, 5H), 2.63 (dd, 2H), 2.56-2.46 (m, 4H), 2.17-0.89 (m, 16H).
WORKUP
后处理
- customto quench
- customthe reaction
- customThe solvent was removed under reduced pressure