تفاعل #2329328

ord-21fbfc68c1b44d2eb08e9d91898f5dec

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture was heated
  2. 2
    درجة الحرارةto reflux overnight
  3. 3
    استخلاصthe mixture was extracted with CH2Cl2 (2×)
  4. 4
    تجفيفThe combined organic layers were dried over Na2SO4
  5. 5
    تركيزconcentrated

الإجراء التجريبي

A solution of trimethylaluminum in heptane (2.0 M, 19.5 mL) was added slowly to a solution of 2-tert-butyl-5-(3,3-dimethoxy-cyclobutyl)-2H-pyrazol-3-ylamine (8.98 g) in CH2Cl2 (60 mL) at room temperature. After 15 min, a solution of 2-methyl-2-pyridin-2-yl-propionic acid ethyl ester (6.85 g) in CH2Cl2 (60 mL) was added. The reaction mixture was heated to reflux overnight. Saturated aqueous NH4Cl solution was added and the mixture was extracted with CH2Cl2 (2×). The combined organic layers were dried over Na2SO4 and concentrated to afford N-[2-tert-butyl-5-(3,3-dimethoxy-cyclobutyl)-2H-pyrazol-3-yl]-2-pyridin-2-yl-isobutyramide as an oil that was used without further purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07671072B2uspto-grants-2010_03