تفاعل #83441

معادلة التفاعل

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

2-methylphenylacetyl chloride

triethylamine

→

desired product

المردود 53.6%

N-[4(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-2-methylbenzeneacetamide

المردود 53.6%

المذيبات

methylene chloride

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued for 72 hours at room temperature
3. 3
   غسيلwashed with water, 2N citric acid, NaCHO3, and brine
4. 4
   تجفيفThe reaction mixture is dried with Na2SO4
5. 5
   ترشيحfiltered through a pad of hydrous magnesium silicate
6. 6
   أخرىevaporated in vacuo
7. 7
   أخرىto give a solid which
8. 8
   أخرىis purified by flash chromatography
9. 9
   أخرىto give a solid which
10. 10
    أخرىis crystallized from ethyl acetate

الإجراء التجريبي

To a stirred solution of 0.334 g of 2-methylphenylacetyl chloride 5 ml of methylene chloride is added 0.346 g of triethylamine at 0° C. After stirring for 3 minutes, 0.500 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added and stirring continued for 72 hours at room temperature. The reaction mixture is diluted with 45 ml of methylene chloride and washed with water, 2N citric acid, NaCHO3, and brine. The reaction mixture is dried with Na2SO4, filtered through a pad of hydrous magnesium silicate and evaporated in vacuo to give a solid which is purified by flash chromatography using 1:1 ethyl acetate-hexane to give a solid which is crystallized from ethyl acetate to give 0.385 g of the desired product as white crystals, m.p. 198°-200° C.

المصدر