反应 #1831909

ord-9b6c71e9e24b44649d2cc73187955e11

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A 500 mL round bottom flask equipped with a mechanical stirrer
  2. 2
    其他After the above mixture was reacted at room temperature for 4 hrs
  3. 3
    其他was carried out at 80° C. for 3.3
  4. 4
    萃取extracted with chloroform (2×150 mL)
  5. 5
    洗涤washed with water (2×100 mL)
  6. 6
    干燥dried with sodium sulfate
  7. 7
    其他The solvent was evaporated
  8. 8
    workup.DISTILLATIONdistilled
  9. 9
    其他to give pure product

实验过程

A 500 mL round bottom flask equipped with a mechanical stirrer was charged with 9.7g (0.075 mol) of 5-norbornene-2-methanol, and 25 ml of DMSO. Potassium hydroxide (7.3g, 85% in purity; 0.13 mol) was added to the above mixture. After the above mixture was reacted at room temperature for 4 hrs., 15.9 g (0.15 mol) of n-octylbromide was slowly added to the above mixture over 25 min. The reaction was carried out at 80° C. for 3.3. hrs. After the reaction mixture was cooled to room temperature, the reaction mixture was combined with water (100 mL), extracted with chloroform (2×150 mL), washed with water (2×100 mL), and dried with sodium sulfate. The solvent was evaporated and the residue was vacuum distilled to give pure product.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07018559B2uspto-grants-2006_03