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
- 0 °C
PROCEDURE
实验过程
Trifluoroacetic acid (3 ml) was added to an ice cooled solution of 1,1-dimethylethyl 6-(5-{3-cyano-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-5-methyl-3,4-dihydro-2(1H)-isoquinolinecarboxylate (Preparation 22; 486 mg, 1.02 mmol) in dichloromethane (3 ml). The reaction mixture was stirred at 0° C. for 30 minutes. The solvent was evaporated and the residue co-evaporated from toluene (×2). Trituration of the residue with diethyl ether gave the title compound as a colourless solid which was filtered off and dried (485 mg). 1H NMR (400 MHz, CDCl3) δ: 1.48 (6H, d), 2.54 (3H, s), 3.09 (2H, m), 3.5 (2H, obscured by residual solvent), 4.36 (2H, s), 4.80 (1H, m), 7.08-7.15 (2H, m), 7.85 (1H, d), 8.33 (1H, d), 8.42 (1H, s), 10.20 (2H, br s). MS m/z 375 [MH]+.
WORKUP
后处理
- customThe solvent was evaporated