반응 #94749

반응 방정식

Na2SO4

LiAlH4

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

LiAlH4

→

2-Amino-1-(3',4'-dimethoxyphenyl)-7-(4'-fluorophenyl)-5-heptanone ethylene ketal

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition the reaction mixture
2. 2
   온도was refluxed gently for 2 hours
3. 3
   여과The inorganic salts were filtered off
4. 4
   세척washed with ether
5. 5
   추출The organic layer was extracted twice with water
6. 6
   건조dried over anh MgSO4
7. 7
   여과filtered
8. 8
   농축concentrated under reduced pressure to 250 ml

실험 절차

To a suspension of 22.0 g (0.58 mole) of LiAlH4 in 400 ml of dry tetrahydrofuran was added dropwise a solution of 84.8 g (0.2 mole) of 1-(3',4'-dimethoxyphenyl)-7-(4'-fluorophenyl)-2-nitro-5-heptanone ethylene ketal in a minimum amount of dry tetrahydrofuran. After the addition the reaction mixture was refluxed gently for 2 hours. The excess LiAlH4 was decomposed with saturated Na2SO4 solution. The inorganic salts were filtered off and washed with ether. The organic layer was extracted twice with water, dried over anh MgSO4, filtered and concentrated under reduced pressure to 250 ml. This was used in the next step.

출처