تفاعل #2348133

ord-fae726d3a9ab40aea603992cbc6ce297

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONAfter the dropwise addition
  2. 2
    أخرىthe resulting reaction solution
  3. 3
    غسيلwas successively washed with 200 ml of water, 200 ml of 2N hydrochloric acid, and 200 ml of a saturated sodium bicarbonate water
  4. 4
    تجفيفwas dried over anhydrous magnesium sulfate
  5. 5
    ترشيحAfter the filtration
  6. 6
    تركيزthe resultant was concentrated

الإجراء التجريبي

Under a nitrogen atmosphere, a solution of 22.8 g (100 mmol) of 3,7,11-trimethyldodecanol and 9.48 g (120 mmol) of pyridine in 200 ml of dry methylene chloride was added dropwise to a solution of 20.96 g (110 mmol) of p-toluenesulfonyl chloride in 100 ml of dry methylene chloride under ice cooling (1 to 2° C.). After the dropwise addition, the resultant was agitated at room temperature overnight, 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 was dried over anhydrous magnesium sulfate. After the filtration, the resultant was concentrated to obtain 41.6 g of crude 3,7,11-trimethyldodecyl tosylate.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07846903B2uspto-grants-2010_12