HRID710490
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 the product of Step D (0.17 g, 0.47 mmol) in a mixture of MeOH and H2O (10 ml: 1 ml), NaHCO3 (0.3 g, 3.6 mmol) was added and the reaction mixture was stirred at reflux for 2 h. The solvents were evaporated and the residue was diluted to 20 ml with EtOAc and washed with H2O, dried over MgSO4, filtered and the filtrate evaporated to dryness to give the title compound (0.12 g; 100%), as pale oil. 1H-NMR (CDCl3) 0.86 (tr, 3H, J=6.93 Hz); 1.25-1.28 (m, 12H), 1.45-1.6 (m, 2H); 2.52 (tr, 2H, J=7.71 Hz); 2.85-2.93 (m, 8H); 6.85-6.92 (m, 2H); 6.97-7.0 (m, 1H).
WORKUP
后处理
- additionwas added
- temperatureat reflux for 2 h
- customThe solvents were evaporated
- additionthe residue was diluted to 20 ml with EtOAc
- washwashed with H2O
- dry with materialdried over MgSO4
- filtrationfiltered
- customthe filtrate evaporated to dryness