تفاعل #3671

معادلة التفاعل

Water

4-[(2-methyl-5-fluorobenzoyl)amino]-2-chlorobenzoyl chloride

10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine

N,N-diisopropylethylamine

→

glass

N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)-3-chlorophenyl]-3-fluoro-2-methylbenzamide

المذيبات

methylene chloride

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةWhile cooling in an ice bath
2. 2
   غسيلthe separated organic layer washed with saturated sodium bicarbonate
3. 3
   تجفيفdried with Na2SO4
4. 4
   أخرىThe methylene chloride is removed in vacuo

الإجراء التجريبي

To a solution of 1.50 g of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 25 ml of methylene chloride is added 1.23 g of N,N-diisopropylethylamine. While cooling in an ice bath, a solution of 3.08 g of [4-[(2-methyl-5-fluorobenzoyl)amino]-2-chlorobenzoyl chloride in 50 ml of methylene chloride is added. The reaction mixture becomes homogeneous and is stirred at room temperature for 18 hours. Water is added and the separated organic layer washed with saturated sodium bicarbonate, dried with Na2SO4 and passed through a short pad of hydrous magnesium silicate two times. The methylene chloride is removed in vacuo to give 3.81 g of a glass. A sample is crystallized from ethyl acetate to give crystalline solid, m.p. 200°-205° C.

المصدر