تفاعل #70451

ord-7373e526e63343878cd0b20258e7f221

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe organic layer is separated
  2. 2
    تجفيفdried over sodium sulfate
  3. 3
    تركيزconcentrated under reduced pressure to a white residue
  4. 4
    أخرىThe solid is further dried under high vacuum

الإجراء التجريبي

Triethylamine (4.13 g, 3 mL, 40.8 mmol, 4 eq) is added to a solution of 6-chloro-nicotinonitrile (1.38 g, 10 mmol, 1 eq), (S)-2-methyl-piperazine (1.00 g, 10 mmol, 1 eq) in DMF (15 mL), and the resulting solution is stirred at rt for 14 h. A white precipitate of triethylamine hydrochloride forms in the course of the reaction. Water (15 mL) and EtOAc (100 mL) are added, the organic layer is separated, dried over sodium sulfate and concentrated under reduced pressure to a white residue. The solid is further dried under high vacuum to yield the desired product as a white solid (1.4 g, 69%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08536168B2uspto-grants-2013_09