تفاعل #75953

ord-d5f1d0d3073d452b8ad7c8c476d8d731

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىresulting two-phase mixture
  2. 2
    استخلاصextracted with ethyl acetate
  3. 3
    غسيلThe combined organic extracts were washed with brine
  4. 4
    تجفيفdried over anhydrous sodium sulfate
  5. 5
    أخرىevaporated

الإجراء التجريبي

A solution of sulfuryl chloride (12.4 mmol) in toluene (5 mL) was added dropwise via an additional funnel to a solution of ethyl isobutyrylacetate (12.4 mmol) in toluene (20 mL) over 5 minutes at room temperature. The resulting mixture was stirred at room temperature overnight. Water was added slowly and resulting two-phase mixture was basified with saturated NaHCO3 and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over anhydrous sodium sulfate, and evaporated to afford 2.2 g (84%) of product as a pale yellow oil: MH+=227.0, retention time (LC-MS)=2.77 min.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06699860B2uspto-grants-2004_03