HRID710490

反应详情

EQUATION

反应方程式

HRID 710490 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. additionwas added
  2. temperatureat reflux for 2 h
  3. customThe solvents were evaporated
  4. additionthe residue was diluted to 20 ml with EtOAc
  5. washwashed with H2O
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customthe filtrate evaporated to dryness