反应 #2343604

ord-00e8e26907d6419b96824ba1fa112a96

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他equipped with a stirrer
  2. 2
    温度This reaction mixture was cooled to 5°±3° C.
  3. 3
    温度was maintained at 5°±3° C
  4. 4
    workup.WAITThe reaction was held at this temperature for an additional hour at which
  5. 5
    workup.ADDITIONwas slowly added with the temperature
  6. 6
    其他kept below 15° C
  7. 7
    洗涤The reaction mixture was then washed 3 times with 5% HCL
  8. 8
    洗涤washed twice with 5% NaOH, once with water, once with dil. HCl, once with water
  9. 9
    其他to give 192.0 g of a light brown, fluid oil

实验过程

96.0 g (0.72 moles) of anhydrous aluminum chloride was added to a 1 L flask equipped with a stirrer, thermometer, and an addition funnel. 250 mL of carbon tetrachloride was added followed by 68.4 g (0.74 moles) of propionyl chloride from a pipette. This reaction mixture was cooled to 5°±3° C. and 153.9 g (0.625 mole) of "soft" dodecylbenzene (Dodane S, produced by Monsanto Chemical Co.) was then added over a 3 hour period while the temperature was maintained at 5°±3° C. The reaction was held at this temperature for an additional hour at which point approximately 500 mL of 10% HCl was slowly added with the temperature kept below 15° C. The reaction mixture was then washed 3 times with 5% HCL, once with water and the solvent stripped under vacuum. The residue was taken up in toluene and washed twice with 5% NaOH, once with water, once with dil. HCl, once with water and then stripped to give 192.0 g of a light brown, fluid oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05654458uspto-grants-1997_08