HRID1075620

反应详情

EQUATION

反应方程式

HRID 1075620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A 3.6% sodium perchlorate solution was added dropwise to a mixture of 5,5,8,8-tetramethyl-5,6,7,8tetrahydronaphthalen-2-ol(6.35 g, 31.1 mmol), sodium hydroxide (1.23 g, 34.2 mmol) and sodium iodide (4.6 g, 31.1 mmol) in methanol (115 ml), at 0° C. The mixture was maintained under stirring for two hours at 0° C. 33 ml of a 10% sodium thiosulfate solution were added. After stirring, the mixture was acidified with hydrochloric acid to pH 1. It was extracted with 200 ml of ethyl ether. The organic phase was washed twice with 400 ml of water, dried over magnesium sulfate and concentrated in a rotary evaporator under vacuum at 40° C.

WORKUP

后处理

  1. temperatureThe mixture was maintained
  2. stirringAfter stirring
  3. extractionIt was extracted with 200 ml of ethyl ether
  4. washThe organic phase was washed twice with 400 ml of water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in a rotary evaporator under vacuum at 40° C.