تفاعل #75628

معادلة التفاعل

1-(3-Bromo-8-chloro-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-yl)-4-[(4-piperidinyl)acetyl]piperazine

methyl isocyanate

methyl isocyanate

→

title compound

المردود 84.8%

4-[2-[4-(3-Bromo-8-chloro-6,11-dihydro-5H-benzo[5,6]-cyclohepta[1,2-b]pyridin-11-yl)-1-piperazinyl]-2-oxoethyl]-N-methyl-1-piperidinecarboxamide

المردود 84.8%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe reaction was stirred for a total of 144 h
2. 2
   درجة الحرارةThe solution was heated at 74° C. for 5 h
3. 3
   workup.STIRRINGthe stirred at 25° C. for an additional 24 h
4. 4
   أخرىThe solution was chromatographed on silica gel using 2% (10% conc. NH4OH in methanol)dichloromethane as the eluant

الإجراء التجريبي

1-(3-Bromo-8-chloro-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-yl)-4-[(4-piperidinyl)acetyl]piperazine (Preparative Example 10) (500 mg, 0.9 mmoles) was dissolved in anhydrous dichloromethane (5 ml) and methyl isocyanate (220.3 mg, 3.6 mmoles) was added. The mixture was stirred under argon at 25° C. for 47 h. Additional methyl isocyanate (110.15 mg, 1.8 mmoles) was added and the reaction was stirred for a total of 144 h. The solution was heated at 74° C. for 5 h and the stirred at 25° C. for an additional 24 h. The solution was chromatographed on silica gel using 2% (10% conc. NH4OH in methanol)dichloromethane as the eluant to give 438.9 mg of the title compound (Yield: 79%).

المصدر