تفاعل #83490

معادلة التفاعل

10,11-dihydro-10-(4-nitro-3-methoxybenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

hydrazine

→

crystals

المردود 67.3%

10,11-Dihydro-10-(4-amino-3-methoxybenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

المردود 67.3%

المذيبات

ethyl alcohol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated on a steam bath for 1 hour
2. 2
   ترشيحThe hot reaction mixture is filtered through diatomaceous earth
3. 3
   أخرىthe filtrate evaporated in vacuo to a residue which
4. 4
   أخرىis partitioned between methylene chloride and water
5. 5
   تجفيفThe organic layer is dried with Na2SO4
6. 6
   workup.ADDITIONHexane is added to the filtrate
7. 7
   درجة الحرارةwhile heating on a steam bath

الإجراء التجريبي

A mixture of 3.24 g of 10,11-dihydro-10-(4-nitro-3-methoxybenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0.35 g of 10% Pd/c and 0.60 g of anhydrous hydrazine in 100 ml of absolute ethyl alcohol and heated on a steam bath for 1 hour. The hot reaction mixture is filtered through diatomaceous earth and the filtrate evaporated in vacuo to a residue which is partitioned between methylene chloride and water. The organic layer is dried with Na2SO4 and passed through a short pad of hydrous magnesium silicate. Hexane is added to the filtrate while heating on a steam bath to give 2 g of crystals, m.p. 184°-185° C.

المصدر