反応 #11999

ord-c353e953aaf34bf5a0978f79193a0a6e

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was obtained
  2. 2
    洗浄was washed with 1 N HCl (2×5 mL)
  3. 3
    乾燥dried over MgSO4
  4. 4
    濃縮concentrated in vacuo

実験手順

Methyl trifluoroacetate (200 μL, 1.99 mmoles) and triethylamine (184 μL, 1.32 mmoles) were added to a suspension of 12-aminododecanoic acid (300 mg, 1.32 mmoles) in methanol (2 mL). After the mixture was stirred vigorously for 18 h, 1 N HCl was added dropwise until the a pH of 2 was obtained. The reaction was added to ethyl acetate (20 mL) was washed with 1 N HCl (2×5 mL), dried over MgSO4, and concentrated in vacuo to yield the amide as a white solid (398 mg, 1.28 mmoles, 97%). LRMS: not performed. 1H NMR: spectrum is consistent with the predicted structure.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07098196B1uspto-grants-2006_08