HRID2192337

反应详情

EQUATION

反应方程式

HRID 2192337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Phenyl-cycloheptanecarboxylic acid (R)-(1-aza-bicyclo[2.2.2]oct-3-yl)ester (Example 14e) (0.79 mmol) and 2-bromo-N-pyridin-2-yl-acetamide (Example 15a) (0.87 mmol) were stirred together in anhydrous MeCN at room temperature for 2.5 days. The reaction mixture was concentrated in vacuo and the yellow solid purified by flash silica gel column chromatography eluting with 2-8% MeOH/dichloromethane to give a tan solid. The solid was dissolved up in refluxing MeCN and the solution was allowed to cool down to room temperature. The resulting crystals were filtered off and washed with a small quantity of cold MeCN to give the title compound (211 mg) as a white crystalline solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe yellow solid purified by flash silica gel column chromatography
  3. washeluting with 2-8% MeOH/dichloromethane
  4. customto give a tan solid
  5. dissolutionThe solid was dissolved up
  6. filtrationThe resulting crystals were filtered off
  7. washwashed with a small quantity of cold MeCN