HRID260015

反应详情

EQUATION

反应方程式

HRID 260015 的结构方程式

PROCEDURE

实验过程

A mixture of 74 g (0.40 moles) of biphenol and 20 g (0.50 moles) of sodium hydroxide in 600 ml of ethanol was refluxed for 1 hour. At reflux temperature 66 g (0.40 moles) of 6-bromohexane were added over a period of 1 hour. The reaction mixture was refluxed for 18 hours and cooled to room temperature, and the precipitate was filtrated. The filtrate was treated with 500 ml of water and the precipitated 4-hexyloxy-4'-hydroxybiphenyl was filtrated and washed with water. After drying 29 g of product were obtained. An additional amount of product was obtained by refluxing the precipitate collected from the reaction mixture with 45 g of potassium hydroxide in 600 ml of ethanol for 3 hours. This mixture was cooled to room temperature and the insoluble dihexyloxybiphenyl filtered off. The clear filtrate was treated with 200 ml of 6N hydrochloric acid and the precipitated 4-hexyloxy-4'-hydroxybiphenyl was filtrated, washed with water, and dried. The yield was 19 g. The total yield was 48 g (44% of theory).

WORKUP

后处理

  1. temperaturewas refluxed for 1 hour
  2. additionwere added over a period of 1 hour
  3. temperatureThe reaction mixture was refluxed for 18 hours
  4. filtrationthe precipitate was filtrated
  5. additionThe filtrate was treated with 500 ml of water
  6. filtrationthe precipitated 4-hexyloxy-4'-hydroxybiphenyl was filtrated
  7. washwashed with water
  8. dry with materialAfter drying 29 g of product
  9. customwere obtained
  10. customAn additional amount of product was obtained
  11. temperatureby refluxing the precipitate
  12. customcollected from the reaction mixture with 45 g of potassium hydroxide in 600 ml of ethanol for 3 hours
  13. temperatureThis mixture was cooled to room temperature
  14. filtrationthe insoluble dihexyloxybiphenyl filtered off
  15. additionThe clear filtrate was treated with 200 ml of 6N hydrochloric acid
  16. filtrationthe precipitated 4-hexyloxy-4'-hydroxybiphenyl was filtrated
  17. washwashed with water
  18. customdried