반응 #1164116

반응 방정식

Sodium hydride

N-(3-nitrophenyl)-β-chloropropionamide

benzene

→

N-(3-nitrophenyl)-2-azetidinone

용매

carbon tetrachloride

반응 조건

후처리

1. 1
   기타The mineral oil is removed
2. 2
   세척by washing the sodium hydride with benzene, and dimethyl sulfoxide (50 ml)
3. 3
   workup.ADDITIONis thereafter slowly added
4. 4
   workup.STIRRINGThe mixture is stirred until no more hydrogen gas evolves
5. 5
   workup.STIRRINGwith stirring
6. 6
   온도while maintaining the temperature of the reaction mixture below about 30°C
7. 7
   workup.ADDITIONAfter the addition
8. 8
   세척the reaction mixture is washed with water and aqueous sodium bicarbonate
9. 9
   건조The washed mixture is then dried over anhydrous magnesium sulfate
10. 10
    여과is filtered

실험 절차

Sodium hydride (0.1 mole; 57% dispersion in mineral oil) is charged into a glass reaction flask. The mineral oil is removed by washing the sodium hydride with benzene, and dimethyl sulfoxide (50 ml) is thereafter slowly added with stirring. The mixture is stirred until no more hydrogen gas evolves. A solution of N-(3-nitrophenyl)-β-chloropropionamide (0.08 mole) in carbon tetrachloride (50 ml) is added dropwise to the reaction flask with stirring while maintaining the temperature of the reaction mixture below about 30°C. After the addition is completed the reaction mixture is allowed to stand at room temperature for a period of about 8 hours. After this time benzene is added and the reaction mixture is washed with water and aqueous sodium bicarbonate. The washed mixture is then dried over anhydrous magnesium sulfate, is filtered, and is stripped of solvents under reduced pressure to yield the desired product N-(3-nitrophenyl)-2-azetidinone as the residue.

출처