反応 #94742

反応方程式

LiAlH4

1-(3,4-dimethoxyphenyl)-2-nitro-7-(4-methylphenyl)-5-heptanone ethylene ketal

LiAlH4

Na2SO4

→

brown oil

収率 96.1%

1-(3',4'-Dimethoxyphenyl)-2-amino-7-(4'-methylphenyl)-5-heptanone ethylene ketal

収率 96.1%

溶媒

THF

THF

反応条件

後処理

1. 1
   workup.ADDITIONcondensor and addition funnel
2. 2
   温度The reaction was refluxed for 2 hours
3. 3
   ろ過the salts filtered
4. 4
   乾燥the organic layer dried over MgSO4
5. 5
   ろ過filtered
6. 6
   濃縮concentrated

実験手順

In a 500 mL 3 necked rb flask equipped with a mechanical stirrer, condensor and addition funnel, a THF solution of 1-(3,4-dimethoxyphenyl)-2-nitro-7-(4-methylphenyl)-5-heptanone ethylene ketal (15.7 g; 0.037 mole) was added slowly to a suspension of LiAlH4 (14.2 g; 0.111 mole) in dry THF. The reaction was refluxed for 2 hours. Excess LiAlH4 was then decomposed with sat. Na2SO4, the salts filtered and the organic layer dried over MgSO4, filtered and concentrated to yield 14.2 g of a brown oil.

出典