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 methyl {4-[({[(4-tert-butylphenyl)amino]carbonyl}{4-[(4-butylphenyl)-ethynyl]benzyl}amino)methyl]phenoxy}acetate (70 mg, 0.11 mmol) in MeOH (1 mL) and THF (1 mL) was added an aqueous solution of NaOH (0.5 mL, 5N) and the resulting mixture was stirred at it for 3 hrs. Then the solvents were removed under reduced pressure. The residue was taken up in EtOAc and washed with an aqueous solution of HCl (1N) and brine. The organic layer was dried over MgSO4 and the solvent was removed to give 46 mg (67%) of the title compound. HPLC, Rt: 5.67 min (purity: 97.4%). 1H NMR (CD3OD) δ: 7.48 (d, J=8.3 Hz, 2H), 7.40 (d, J=7.5 Hz, 2H), 7.18-7.33 (m, 10H), 6.93 (d, J=8.7 Hz, 2H), 4.66 (s, 2H), 4.66 (s, 2H), 4.54 (s, 2H), 2.63 (t, J=7.5 Hz, 2H), 1.60 (m, 2H), 1.37 (m, 2H), 1.30 (s, 9H), 0.95 (t, J=7.2 Hz, 3H). M+(ESI): 603.4, M−(ESI): 601.3.
WORKUP
后处理
- customThen the solvents were removed under reduced pressure
- washwashed with an aqueous solution of HCl (1N) and brine
- dry with materialThe organic layer was dried over MgSO4
- customthe solvent was removed