HRID1272265

反应详情

EQUATION

反应方程式

HRID 1272265 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of phosphorous oxychloride (1.35 g, 8.8 mmole) and dry pyridine (12 mL) cooled to 0° C., a solution of 3,5-diisopropyl salicylamide (1.10 g, 5 mmole) and dry pyridine (5 mL) was slowly added drop by drop. The reaction mixture was stirred at room temperature, whereat the colour changed from colourless over violet to red. After extraction with ethyl acetate and washing with a saturated sodium chloride solution and 2N hydrochloric acid, the organic layer was dried and evaporated under reduced pressure. The obtained solid residue was recrystallized from acetonitrile, whereat there were obtained 610 mg (60%) of 2-hydroxy-3,5-diisopropyl benzonitrile.

WORKUP

后处理

  1. extractionAfter extraction with ethyl acetate
  2. washwashing with a saturated sodium chloride solution and 2N hydrochloric acid
  3. customthe organic layer was dried
  4. customevaporated under reduced pressure
  5. customThe obtained solid residue was recrystallized from acetonitrile, whereat there