反应 #1118678

ord-a578c95886894db4bfb6f0a295f271a4

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was refluxed for 1 h
  2. 2
    其他quenched by the sequential addition of 2 mL of H2O, 2 mL of 15% aqueous NaOH and finally 6 mL of H2O
  3. 3
    过滤The resulting slurry was filtered
  4. 4
    洗涤the filter cake was washed with additional tetrahydrofuran
  5. 5
    其他Evaporation of the filtrate

实验过程

To a suspension of LiAlH4 (2.0 g, 0.052 mol) in 50 mL of dry tetrahydrofuran was added dropwise a solution of methyl 1-methylindole-3-acetate (5.25 g, 0.026 mol) in 70 mL of dry tetrahyqrofuran at -10° C. under Ar. The mixture was refluxed for 1 h and then it was cooled at 0° C. and quenched by the sequential addition of 2 mL of H2O, 2 mL of 15% aqueous NaOH and finally 6 mL of H2O. The resulting slurry was filtered and the filter cake was washed with additional tetrahydrofuran. Evaporation of the filtrate gave the product (40 g, 89%) as an oil which was used without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04954502uspto-grants-1990_09