تفاعل #1436

معادلة التفاعل

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

المذيبات

methyl alcohol

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر