反応 #1447123

ord-cb8e894fb6f642e68ae41001b4f15a85

反応方程式

CC(C)CC(=O)c1ccccc1N
1-(2-aminophenyl)-3-methylbutan-1-one
NN.O
hydrazine hydrate
O
water
[K+].[OH-]
potassium hydroxide
CC(C)CCc1ccccc1N
[2-(3-methylbutyl)-phenyl]amine
収率 72.1%

反応条件

温度
210°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The organic phase is again washed with water
  2. 2
    乾燥dried over magnesium sulphate
  3. 3
    濃縮concentrated under reduced pressure
  4. 4
    その他Purification by column chromatography (cyclohexane/ethyl acetate 3:1)

実験手順

A solution comprising 8.0 g (0.045 mol) of 1-(2-aminophenyl)-3-methylbutan-1-one (X-1), 6.8 g (0.135 mol) of hydrazine hydrate and 7.6 g (0.135 mol) of potassium hydroxide in 90 ml of triethylene glycol is heated at 210° C. for 6 h. For work-up, water and ethyl acetate are added at room temperature. The organic phase is again washed with water, dried over magnesium sulphate and concentrated under reduced pressure. Purification by column chromatography (cyclohexane/ethyl acetate 3:1) gives 5.3 g (71.5% of theory) of [2-(3-methylbutyl)-phenyl]amine.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07879760B2uspto-grants-2011_02