反応 #11540

ord-f6144ee0e8f24ce288490dbd6a6d4c57

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture was refluxed overnight
  2. 2
    洗浄washed with hexane (100 ml)
  3. 3
    その他to remove sodium hydride oil
  4. 4
    濃縮concentrated under reduced pressure
  5. 5
    ろ過The resulting crystals were filtered off with ethyl acetate

実験手順

Next, 6 N hydrochloric acid (96.8 ml, 581 mmol) was added to diethyl 2-methyl-2-(4-pyridylmethyl)malonate (17.2 g, 64.6 mmol), and the mixture was refluxed overnight. The reaction mixture was allowed to stand, then washed with hexane (100 ml) to remove sodium hydride oil contained in diethyl 2-methyl-2-(4-pyridylmethyl)malonate, and concentrated under reduced pressure. The resulting crystals were filtered off with ethyl acetate to give 10.7 g (82%) of 2-methyl-3-(4-pyridyl)propionic acid as pale pink crystals.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07098226B2uspto-grants-2006_08