HRID1706937

反应详情

EQUATION

反应方程式

HRID 1706937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To the solution containing 1.25 g. of farnesyl carboxylic acid dissolved in 0.5 N ammonia water, 0.845 g. of silver nitrate in 3 ml. water was added. The resulting precipitate was collected by filtration and dried. The silver salt was powdered and suspended in 120 ml. of benzene, and distilled to about 60 ml. of benzene solution to remove the remaining water azeotropically. Separately, α-bisabolol chloride was prepared by adding triphenyl phosphine in an amount of 1.3 times the stoichiometric quantity, to α-bisabolol in a solution of carbon tetrachloride (1:8) and following 1 hour of reflux in water bath, the product was purified by vacuum distillation. The purified α-bisabolol chloride in an amount of 1.39 g. was dissolved in 3 ml. of benzene and added to the above solution of silver salt suspension which had been prepared previously. After 9 hours of reflux, the reaction mixture was washed with water and dried (sodium sulfate). The desired fraction was obtained by vacuum distillation (155°-156° C./0.1 mmHg) under N2 gas stream.

WORKUP

后处理

  1. additionTo the solution containing 1.25 g
  2. filtrationThe resulting precipitate was collected by filtration
  3. customdried
  4. distillationof benzene, and distilled to about 60 ml
  5. customof benzene solution to remove the remaining water azeotropically
  6. distillationthe product was purified by vacuum distillation
  7. dissolutionwas dissolved in 3 ml
  8. additionof benzene and added to the above solution of silver salt suspension which
  9. customhad been prepared previously
  10. temperatureAfter 9 hours of reflux
  11. washthe reaction mixture was washed with water
  12. dry with materialdried (sodium sulfate)
  13. customThe desired fraction was obtained by vacuum distillation (155°-156° C./0.1 mmHg) under N2 gas stream