تفاعل #61549

ord-9dfa7266ae6b456696c440543ead31df

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGThe reaction was stirred at room temperature for 2 h
  2. 2
    استخلاصthe mixture was extracted with DCM (3×100 ml)
  3. 3
    تجفيفThe combined organic layers were dried over MgSO4
  4. 4
    ترشيحfiltered
  5. 5
    تركيزconcentrated under reduced pressure
  6. 6
    أخرىThe product was used in the next reaction step without further purification

الإجراء التجريبي

To a solution of 1 g 5-[2-(2-Methoxy-ethoxy)-ethoxy]-2H-pyrazole-3-carboxylic acid ethyl ester in 10 ml of DMF and 154 mg of sodium hydride (60% in mineral oil) were added at RT. After stirring for 5 min at room temperature, 966 mg of 2-Bromo-N-(5-chloro-pyridin-2-yl)-acetamide were added. The reaction was stirred at room temperature for 2 h. Then 50 ml of water were added and the mixture was extracted with DCM (3×100 ml). The combined organic layers were dried over MgSO4, filtered and concentrated under reduced pressure. The product was used in the next reaction step without further purification. Yield: 1.2 g.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07429581B2uspto-grants-2008_09