تفاعل #157154

ord-a0266f5e87fd437b9ef457e73767b91a

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةUpon cooling to room temperature
  2. 2
    استخلاصthe mixture was extracted with EtOAc
  3. 3
    تجفيفdried with Na2SO4
  4. 4
    تركيزconcentrated
  5. 5
    أخرىThe crude material was purified via SiO2 column chromatography
  6. 6
    غسيلeluting with DCM/MeOH (2%)

الإجراء التجريبي

To a solution of 4,6-dichloropyridin-2-amine (1.0 equiv.) in THF (0.1M) was added Pd(dppf)Cl2-DCM (0.1M), K2CO3 (3.0 equiv.), and Et2Zn (1.2 equiv.). The reaction was heated to 70° C. for 18 hrs. Upon cooling to room temperature, NH4Cl(sat.) was added, the mixture was extracted with EtOAc, dried with Na2SO4, and concentrated. The crude material was purified via SiO2 column chromatography eluting with DCM/MeOH (2%) to yield 4-chloro-6-ethylpyridin-2-amine in 33% yield. LCMS (m/z): 157.1 (MH+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08822497B2uspto-grants-2014_09