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
CDl (194.4 mg, 1.2 mmol) is added to the solution of 4-(2-hydroxyhexafluoroisopropyl) benzoic acid (288 mg, 1 mmol) in THF (10 mL) at room temperature. The reaction mixture is stirred for 10 minutes and N-methylphenethylamine (0.174 mL, 1.2 mmol) is introduced. The reaction mixture is then stirred for 14 hours. The solvent is removed and the residue is dissolved in EtOAc. The organic phase is washed with 1N HCl, saturated NaHCO3 and brine and dried over MgSO4. The product is obtained in pure form after removal of solvents (278.8 mg). 1H NMR (CD3OD, every peak appears as a pair) δ2.76 (t, 2H), 3.12 (s, 3H), 3.44 (t, 2H), 7.01 (d, 2H), 7.20 (d, 2H), 7.30 (m, 3H), 7.62 (d, 2H); ESIMS: m/z 406 (M+H).
WORKUP
后处理
- stirringThe reaction mixture is then stirred for 14 hours
- customThe solvent is removed
- dissolutionthe residue is dissolved in EtOAc
- washThe organic phase is washed with 1N HCl, saturated NaHCO3 and brine
- dry with materialdried over MgSO4
- customThe product is obtained in pure form
- customafter removal of solvents (278.8 mg)