تفاعل #92063

ord-0f6fd8b006f14602ba848464c8fc3fcd

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGstirred at room temperature for 10 minutes
  2. 2
    أخرىThe organic layer was separated
  3. 3
    تجفيفdried over anhydrous sodium sulfate
  4. 4
    تركيزconcentrated
  5. 5
    أخرىseparated through a short column with ethyl acetate

الإجراء التجريبي

In an ice bath, 29.8 g of pivaloyl chloride (226 mmol) was added dropwise to a solution of compound 5 (50.0 g, 207 mmol) and triethylamine (37.9 mL) in dichloromethane (300.0 mL) within one hour and then stirred for 2 hours until the starting materials disappeared. 150 mL of water was added into the reaction solution and stirred at room temperature for 10 minutes. The organic layer was separated, dried over anhydrous sodium sulfate, concentrated, and separated through a short column with ethyl acetate to give white solid (57.7 g, 85.6%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09447101B2uspto-grants-2016_09