反应 #927245

ord-f6c0f997f4574b7d99e3a5984f3dc778

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤the reaction mixture was washed with water (2×) and brine
  2. 2
    干燥dried over magnesium sulfate
  3. 3
    workup.DISSOLUTIONThe product was dissolved in 70 ml of THF
  4. 4
    温度refluxed for 8 hours with an additional 25 g of lithium bromide

实验过程

1-Bromodec-4-yne was prepared from 1-chlorodec-4-yne. The 1-chlorodec-4-yne (10.6 g, 61 mmol) and 25 g of lithium bromide were refluxed in 80 ml of THF for 21 hours. The conversion was 74%. Ether was added, the reaction mixture was washed with water (2×) and brine, dried over magnesium sulfate and stripped. The product was dissolved in 70 ml of THF and refluxed for 8 hours with an additional 25 g of lithium bromide. This gave 95% conversion of the chloride to the bromide. The same workup provided 11.36 g of 1-bromodec-4-yne.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06365549B2uspto-grants-2002_04