反応 #1106681

ord-e312b6e2b9cd415fa3d6eed75d8565e7

反応方程式

NC(=O)C1Oc2ccccc2O1
Benzo[1,3]dioxole-2-carboxylic acid amide
[Al+3].[H-].[H-].[H-].[H-].[Li+]
Lithium aluminum hydride
O
water
NCC1Oc2ccccc2O1
C-benzo[1,3]dioxol-2-yl-methylamine

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他to destroy the excess LAH
  2. 2
    workup.ADDITIONAqueous sodium hydroxide (3.0 M, 100 mL) was added
  3. 3
    抽出the solution was extracted with ethyl acetate (3×100 mL)
  4. 4
    洗浄The combined organic solution was washed with water
  5. 5
    乾燥dried over MgSO4
  6. 6
    その他The solvent was evaporated

実験手順

Benzo[1,3]dioxole-2-carboxylic acid amide (5.44 g, 32.9 mmol) was dissolved in tetrahydrofuran (THF, 100 mL). Lithium aluminum hydride (LAH, 1M in THF, 39.5 mL, 39.5 mmol) was added slowly to the solution at room temperature. The reaction was stirred at room temperature for 24 hours. Distilled water was added to destroy the excess LAH. Aqueous sodium hydroxide (3.0 M, 100 mL) was added and the solution was extracted with ethyl acetate (3×100 mL). The combined organic solution was washed with water and dried over MgSO4. The solvent was evaporated to yield C-benzo[1,3]dioxol-2-yl-methylamine as a colorless oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08716231B2uspto-grants-2014_05