HRID2287202

反应详情

EQUATION

反应方程式

HRID 2287202 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The product from step (b) (200 mg; 0.61 mmole) in potassium hydroxide dried pyridine (5 ml) was heated on a steam bath with anhydrous lithium iodide (1 g; 7.5 mmole) for 1 hour. The mixture was cooled and concentrated hydrochloric acid diluted with an equal volume of water was added until the resulting suspension was at pH2. The product was extracted with ethylacetate, washed with water and dried (anhydrous sodium sulphate) to yield a red solid which was recrystallised from ethanol to give the title compound as red crystals (160 mg; 80%) mp 244° (decomposition).

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. additionwas added until the resulting suspension
  3. extractionThe product was extracted with ethylacetate
  4. washwashed with water
  5. dry with materialdried (anhydrous sodium sulphate)
  6. customto yield a red solid which
  7. customwas recrystallised from ethanol