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
A solution of 2-(4-{3-[1-(3,4-dimethyl-benzyl)-2,5-dioxo-imidazolidin-4-yl]-propyl}-phenoxy)-2-methyl-propionic acid tert-butyl ester (0.113 g, 0.228 mmol) in THF (6 mL) was treated dropwise with 1 M solution of borane-THF complex in THF (4.4 mL, 4.4 mmol) and then stirred at room temperature under N2 for 32 h. The reaction was quenched with methanol (6 mL) and stirred at room temperature for 2 hr. The solvent was removed in vacuo to give crude product that was purified by flash chromatography using 97:3 CH2Cl2:MeOH to afford 0.051 g (47%) 2-(4-{3-[1-(3,4-dimethyl-benzyl)-2-oxo-imidazolidin-4-yl]-propyl}-phenoxy)-2-methyl-propionic acid tert-butyl ester. MS (ES+) Calc'd for C29H41N2O4 (M+1) 481. Found m/z 481 (100%). 1H NMR.
WORKUP
后处理
- customThe reaction was quenched with methanol (6 mL)
- stirringstirred at room temperature for 2 hr
- customThe solvent was removed in vacuo
- customto give crude product that
- customwas purified by flash chromatography