HRID2244219

反应详情

EQUATION

反应方程式

HRID 2244219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 20 mL of thionyl chloride was added 0.244 g (0.001 mol) of 2′-(methylthio)-1,1′-biphenyl-4-carboxylic acid of Step A. The solution was heated under reflux for 1 hour. The excess thionyl chloride was removed in a vacuo. To the residue was added 25 mL of dry pyridine and 0.318 g (0.001 mol) of N-(pyridyl-3-ylmethyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxamide of Example 12. The reaction was allowed to stand at room temperature for 1 hour and the pyridine was removed in vacuo. The residue was collected and washed with water giving a tan solid (0.62 g), m.p. 172-175° C.

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureunder reflux for 1 hour
  3. customThe excess thionyl chloride was removed in a vacuo
  4. customthe pyridine was removed in vacuo
  5. customThe residue was collected
  6. washwashed with water giving a tan solid (0.62 g), m.p. 172-175° C.