反応 #1436

反応方程式

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

溶媒

methyl alcohol

反応条件

後処理

1. 1
   workup.ADDITIONwas added to the resulting solution
2. 2
   その他After completion of the hydrogen absorption
3. 3
   ろ過the reaction solution was filtered
4. 4
   濃縮concentrated
5. 5
   workup.DISSOLUTIONThe thus obtained residue was dissolved in dichloromethane
6. 6
   洗浄washed with a saturated sodium bicarbonate aqueous solution
7. 7
   乾燥The resulting dichloromethane layer was dried over anhydrous magnesium sulfate
8. 8
   濃縮concentrated under a reduced pressure
9. 9
   その他The thus obtained residue was recrystallized from methyl alcohol

実験手順

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.

出典