HRID2261876

反应详情

EQUATION

反应方程式

HRID 2261876 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

87.3 g of trans-2-[4-(4-chlorophenyl)cyclohexyl]-3-chloro-1,4-naphthoquinone (trans-isomer of Formula IV) as obtained in Example 7 was suspended in 2619 ml methanol. 128 g potassium hydroxide was dissolved in 873 ml water and added drop-wise to the suspension under heating over a period of 20 minutes. Refluxed was extended for another 45 minutes before cooling to 0-5° C. and filtered. The filtrate was acidified with 50% aqueous hydrochloric acid to precipitate the product. The precipitated product was filtered, and recrystallized from acetonitrile to obtain 71.6 g (86% yield) atovaquone.

WORKUP

后处理

  1. additionadded drop-wise to the suspension
  2. temperatureunder heating over a period of 20 minutes
  3. temperatureRefluxed
  4. filtrationfiltered
  5. customto precipitate the product
  6. filtrationThe precipitated product was filtered
  7. customrecrystallized from acetonitrile