تفاعل #85806

ord-1d1e0032d13f4159b2fc306ea574db4d

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
-72°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONAfter the completion of the addition
  2. 2
    درجة الحرارةslowly warmed up
  3. 3
    workup.STIRRINGstirred at the ambient temperature overnight
  4. 4
    أخرىthe volatiles were removed under reduced pressure

الإجراء التجريبي

A solution of 5-bromo-N,N-dimethylpyridin-2-amine (500 mg, 2.5 mmol) in THF (10 mL) was treated with n-BuLi (1.2 mL, 3 mmol) at −72° C. for 2 hours. Triisopropyl borate (705 mg, 3.75 mmol) was then added dropwise. After the completion of the addition, the mixture was stirred at −72° C. for an additional 1 hour and slowly warmed up and stirred at the ambient temperature overnight. MeOH was carefully added, and the volatiles were removed under reduced pressure to give the title compound. MS (m/z): 167 (M+H)+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09434726B2uspto-grants-2016_09