반응 #1436

반응 방정식

1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro1H-1-benzazepin-5-one

dimethylformamide

→

1-(4-aminobenzoyl)-2,3,4,5-tetrahydro1H-1-benzazepin-5-one

용매

methyl alcohol

반응 조건

후처리

1. 1
   workup.ADDITIONwas added to the resulting solution
2. 2
   기타After completion of the hydrogen absorption
3. 3
   여과the reaction solution was filtered
4. 4
   농축concentrated
5. 5
   workup.DISSOLUTIONThe thus obtained residue was dissolved in dichloromethane
6. 6
   세척washed with a saturated sodium bicarbonate aqueous solution
7. 7
   건조The resulting dichloromethane layer was dried over anhydrous magnesium sulfate
8. 8
   농축concentrated under a reduced pressure
9. 9
   기타The thus obtained residue was recrystallized from methyl alcohol

실험 절차

A 19.2 g portion of 1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro1H-1-benzazepin-5-one was dissolved in a mixed solvent consisting of 200 ml of dimethylformamide and 100 ml of methyl alcohol, and 3 ml of Raney nickel was added to the resulting solution to carry out hydrogenation at normal pressure. After completion of the hydrogen absorption, the reaction solution was filtered and concentrated. The thus obtained residue was dissolved in dichloromethane and then washed with a saturated sodium bicarbonate aqueous solution. The resulting dichloromethane layer was dried over anhydrous magnesium sulfate and then concentrated under a reduced pressure. The thus obtained residue was recrystallized from methyl alcohol to obtain 15.5 g of 1-(4-aminobenzoyl)-2,3,4,5-tetrahydro1H-1-benzazepin-5-one.

출처