反应 #2348136

ord-12bbe2fe0da44f7ebf1496149f636703

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他from exceeding 10° C
  2. 2
    workup.ADDITIONAfter the completion of addition, agitation
  3. 3
    其他the resulting reaction solution
  4. 4
    洗涤was successively washed with 200 ml of water, 200 ml of 2N hydrochloric acid, and 200 ml of a saturated sodium bicarbonate water
  5. 5
    干燥dried over anhydrous magnesium sulfate
  6. 6
    过滤After the filtration
  7. 7
    浓缩the resultant was concentrated under reduced pressure

实验过程

Under a nitrogen atmosphere, 29.16 g (97.67 mmol) of phytanol and 9.27 g (117.2 mmol) of pyridine were dissolved in 220 ml of dry methylene chloride, and 20.48 g (107.4 mmol) of p-toluenesulfonyl chloride was added little by little under ice cooling, in order to prevent the liquid temperature from exceeding 10° C. After the completion of addition, agitation was continued for 12 hours until phytanol disappeared, the resulting reaction solution was successively washed with 200 ml of water, 200 ml of 2N hydrochloric acid, and 200 ml of a saturated sodium bicarbonate water, and dried over anhydrous magnesium sulfate. After the filtration, the resultant was concentrated under reduced pressure to obtain 61.31 g of phytanyl tosylate.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07846903B2uspto-grants-2010_12