HRID2417332

反应详情

EQUATION

反应方程式

HRID 2417332 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7 g (24.7 mmol) of 3-bromo-2-hydroxy-5,6,7,8-tetrahydro-5,5,8,6-tetramethylnaphthalene and 40 ml of DMF are introduced into a three-necked flask under a stream of nitrogren. 890mg (29.6 mmol) of sodium hydride (80% in oil) are added portionwise and the mixture is stirred until the evolution of gas has ceased. 1.7 ml (27 mmol) of iodomethane are then added and the mixture is stirred at room temperature for one hour. The reaction medium is poured into water and extracted with ethyl ether, and the organic phase is separated out after settling has taken place, dried over magnesium sulphate and evaporated. 7.3 g (99%) of the expected product are collected in the for of an oil which crystallizes slowly. Melting point 77-8° C.

WORKUP

后处理

  1. stirringthe mixture is stirred at room temperature for one hour
  2. extractionextracted with ethyl ether
  3. customthe organic phase is separated out after settling
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. custom7.3 g (99%) of the expected product are collected in the for of an oil which
  7. customcrystallizes slowly