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 stirred solution of 2′-cyano-5-((2,2-dimethyl-1,3-dioxolan-4-yl)methoxy)-4′-methylbiphenyl-3-carboxylic acid (63 mg, 0.17 mmol) in THF (3 mL) was added 1 M of aq. HCl solution (3 mL, 3 mmol). The reaction mixture was stirred at room temperature for 4 hours, and then concentrated in vacuo. The residue was treated with water and extracted with EtOAc. The combined organic layers were dried over anhydrous MgSO4 and concentrated to afford the title compound. 1H NMR (CD3OD, 400 MHz): 7.77 (t, 1H, J=1.6 Hz), 7.67 (m, 2H), 7.58 (dd, 1H, J=8.0, 2.0 Hz), 7.51 (d, 1H, J=8.0 Hz), 7.38 (t, 1H, J=2.0 Hz), 4.19 (dd, 1H, J=9.6, 4.0 Hz), 4.10 (dd, 1H, J=9.6, 6.0 Hz), 4.02 (m, 1H), 3.72 (dd, 1H, J=11.2, 5.6 Hz), 3.67 (dd, 1H, J=11.2, 5.6 Hz), 2.45 (s, 3H).
WORKUP
后处理
- concentrationconcentrated in vacuo
- additionThe residue was treated with water
- extractionextracted with EtOAc
- dry with materialThe combined organic layers were dried over anhydrous MgSO4
- concentrationconcentrated