HRID1594853

反应详情

EQUATION

反应方程式

HRID 1594853 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1.6 M n-BuLi in hexane (3.38 mL, 5.42 mmol) at 0° C. was added a solution of 2,2,6,6-tetramethyl piperidine (0.91 mL, 5.42 mmol) in anh. THF (10 mL) over 5 min. A solution of 3-(3-methoxy-phenyl)-1-methyl-azepan-2-one (as described in Example 4, Step A) (0.632 g, 2.71 mmol) in anhydrous THF (10 mL) was added and stirred OC for 1 h. Iodomethyl methyl ether (0.275 mL, 3.25 mmol) was added. After stirring for 30 min, the reaction was quenched with H2O, concentrated in vacuo, diluted with EtOAc, washed with 5N HCl (100 mL), water and brine. The organic layer was dried (MgSO4) and concentrated to give the title compound.

WORKUP

后处理

  1. stirringAfter stirring for 30 min
  2. customthe reaction was quenched with H2O
  3. concentrationconcentrated in vacuo
  4. additiondiluted with EtOAc
  5. washwashed with 5N HCl (100 mL), water and brine
  6. dry with materialThe organic layer was dried (MgSO4)
  7. concentrationconcentrated