تفاعل #81410

ord-ea54b1f13fea410ab51f39809f353352

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىPrepared in analogy with a method in Hussey
  2. 2
    أخرىTo a 500 mL round-bottomed flask equipped with nitrogen inlet
  3. 3
    أخرىThe organic layer was separated
  4. 4
    غسيلwashed again with saturated aqueous sodium bicarbonate solution
  5. 5
    تجفيفdried over sodium sulfate
  6. 6
    أخرىevaporated to a yellow oil, 41 grams (100%), as a mixture of diastereomers which

الإجراء التجريبي

Prepared in analogy with a method in Hussey, A. S. and Herr, R. R., J. Org. Chem., 24, 843 (1959). To a 500 mL round-bottomed flask equipped with nitrogen inlet were added 33.3 grams (0.177 tool) of 4-(2-methylphenyl)cyclohexanone and 200 mL methylene chloride. To the stirring solution was added dropwise over 30 minutes a solution of 17.1 mL (0.212 mol) sulfuryl chloride in 10 mL methylene chloride. The reaction was stirred 14 hours at room temperature and poured into saturated aqueous sodium bicarbonate solution. The organic layer was separated, washed again with saturated aqueous sodium bicarbonate solution, dried over sodium sulfate, and evaporated to a yellow oil, 41 grams (100%), as a mixture of diastereomers which was used directly in the next step.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05618811uspto-grants-1997_04