تفاعل #70453

ord-bc5f400ac57641de862139b65cf0bb17

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىMicrowave reaction mixture for 30 min at 150° C
  2. 2
    أخرىPartition between ethyl acetate and water
  3. 3
    أخرىcollecting organic phase
  4. 4
    تجفيفDry with sodium sulfate
  5. 5
    ترشيحfilter
  6. 6
    تركيزconcentrate
  7. 7
    أخرىPurify on preparative HPLC

الإجراء التجريبي

Combine (2S,5R)-2,5-dimethyl-piperazine (200 mg, 1.75 mmol), 6-chloro-nicotinonitrile (1.75 mmol) and triethylamine (5.25 mmol) in a 0.875 M solution of 1-methyl-2-pyrrolidinone. Microwave reaction mixture for 30 min at 150° C. Partition between ethyl acetate and water, collecting organic phase. Wash aqueous layer again with ethyl acetate and combine organics. Dry with sodium sulfate, filter and concentrate. Purify on preparative HPLC to give the title compound. (9% yield)

المصدر

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