反応 #42437

ord-ec36e4517aeb4f9583456d798cf68415

反応条件

温度
40°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度then cooled to room temperature
  2. 2
    その他partitioned between water and ethyl acetate
  3. 3
    その他the layers were separated
  4. 4
    洗浄The organic layer was washed three times with brine
  5. 5
    乾燥dried over anhydrous sodium sulfate
  6. 6
    濃縮concentrated

実験手順

To a mixture of methyl 1-butyl-1H-indole-6-carboxylate, (2.1 g) in glacial acetic acid (25 mL) was added sodium cyanoborohydride (2.28 g). The mixture was heated at 40° C. for 3 h then cooled to room temperature, partitioned between water and ethyl acetate and the layers were separated. The organic layer was washed three times with brine, dried over anhydrous sodium sulfate and concentrated to give 1.64 g of the title compound: 1H NMR (CDCl3) δ 0.969, 1.43, 1.59, 2.99, 3.1, 3.4, 3.88, 7.07, 7.34.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07727997B2uspto-grants-2010_06