反応 #86328

ord-bee313cd09ff46b5a63b767a5a819676

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction mixture was subsequently purified via preparative HPLC
  2. 2
    洗浄eluting with a gradient of 20-70% ACN in H2O (containing 10 mM NH4HCO3)

実験手順

A mixture of 5-bromo-1,2-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid (70 mg, 0.284 mmol), 1-methylpiperazine (28.5 mg, 0.284 mmol), Et3N (0.1 mL) and 2-(1H-benzo[d][1,2,3]triazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate(V) (108 mg, 0.284 mmol) in DMF (3 mL) was stirred at room temperature for 2 hours. The reaction mixture was subsequently purified via preparative HPLC, eluting with a gradient of 20-70% ACN in H2O (containing 10 mM NH4HCO3) to give the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09434743B2uspto-grants-2016_09