HRID710453
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 the product of Step E (0.21 g; 0.5 mmol) in MeOH (10 ml) was added NaOH (0.1 g) and this was stirred for 3 h at room temperature. The solvent was evaporated to dryness and the residue was taken in a mixture of solvents (EtOAc:MeOH:AcOH; 10 ml:2 ml:0.5 ml) and passed through Celite bead, which was washed with EtOAc (10 ml). The combined filtrates were evaporated to dryness to give the title compound (0.145 g, 94%) as pale paste. 1H-NMR (CDCl3) 1.36 (d, 6H, J=6 Hz); 1.74 (5, 6H); 2.04 (s, 3H, 2.1 (s, 6H); 2.43 (s, 3H); 2.72-2.81 (m, 4H); 4.55-4.63 (m, 1H); 6.74 (d, 1H, J=8.25 Hz); 6.94 (dd, 1H, J=1.97, 8.18 Hz); 7.01 (d, 1H, J=1.98 Hz).
WORKUP
后处理
- customThe solvent was evaporated to dryness
- additionthe residue was taken in a mixture of solvents (EtOAc:MeOH:AcOH; 10 ml:2 ml:0.5 ml)
- washwas washed with EtOAc (10 ml)
- customThe combined filtrates were evaporated to dryness