تفاعل #3695
ord-cc4b68ef8db8421b815156d3cb52f80e
معادلة التفاعل
ethyl 10,11-dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxylate
N,N-diisopropylethylamine
2,4-dichlorobenzoyl chloride
→
solid
المردود 55.4%
Ethyl 10-[4-[(2,4-dichlorobenzoyl)amino]-3-methylbenzoyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]-benzodiazepine-3-carboxylate
المردود 55.4%
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1غسيلwashed with water, saturated NaHCO3
- 2تجفيفdried with Na2SO4
- 3workup.ADDITIONHexane is added to the filtrate at the boil
الإجراء التجريبي
To a solution of 0.30 g of ethyl 10,11-dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxylate in 20 ml of methylene chloride is added 0.15 g of N,N-diisopropylethylamine and 0.24 g of 2,4-dichlorobenzoyl chloride. The reaction mixture is stirred at room temperature for 18 hours and washed with water, saturated NaHCO3 and dried with Na2SO4. The organic layer is passed through a pad of hydrous magnesium silicate. Hexane is added to the filtrate at the boil to give 0.24 g of solid, m.p. 174°-184° C.