تفاعل #1563932

ord-3217d26f18624a8fb770ca68ae0c2486

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITwas continued at 10° C. for 2 h
  3. 3
    أخرىReaction mixture
  4. 4
    أخرىwas quenched with saturated NH4Cl solution
  5. 5
    استخلاصextracted with EtOAc
  6. 6
    تجفيفdried over anhydrous sodium sulphate
  7. 7
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

2.0 M Isopropyl magnesium chloride solution in THF (163 mL, 324.3 mmol) was added to a solution of 2-bromo-1,4-difluorobenzene (62.5 g, 324.3 mmol) in THF (350 mL) at −40° C. and stirring was continued at 5° C. for 1 h. tert-Butyl 2-oxopyrrolidine-1-carboxylate (Step-1) (73 g, 392 mmol) in THF (150 mL) was added dropwise to above reaction mixture at −40° C. and stirring was continued at 10° C. for 2 h. Reaction mixture was quenched with saturated NH4Cl solution, extracted with EtOAc, dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford 76 g of the title compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09402833B2uspto-grants-2016_08