تفاعل #3647

ord-b2aca09294cd4507a7fd38eab4bba6a8

معادلة التفاعل

Cc1ccccc1C(=O)Cl
2-methylbenzoyl chloride
CCN(CC)CC
triethylamine
Nc1ccc(C(=O)N2Cc3cccn3Cc3sccc32)cc1
4,10-dihydro-4-(4-aminobenzoyl)-5H-pyrrolo-[1,2-a]thieno[3,2-e][1,4]diazepine
Cc1ccccc1C(=O)Nc1ccc(C(=O)N2Cc3cccn3Cc3sccc32)cc1
desired product
Cc1ccccc1C(=O)Nc1ccc(C(=O)N2Cc3cccn3Cc3sccc32)cc1
N-[4-(5H-Pyrrolo[1,2-a]thieno[3,2-e][1,4]diazepin-4(10H)-ylcarbonyl)phenyl]-2-methylbenzamide

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلThe reaction mixture is washed with water, 2N citric acid, NaHCO3, and brine
  2. 2
    تجفيفThe reaction mixture is dried with Na2SO4
  3. 3
    ترشيحfiltered
  4. 4
    أخرىevaporated in vacuo
  5. 5
    أخرىto give a solid which
  6. 6
    أخرىis purified by flash chromatography on silica gel

الإجراء التجريبي

To a stirred solution of 3 mmol of 2-methylbenzoyl chloride in 10 ml of methylene chloride is added 5 mmol of triethylamine and 3 mmol of 4,10-dihydro-4-(4-aminobenzoyl)-5H-pyrrolo-[1,2-a]thieno[3,2-e][1,4]diazepine. The mixture is stirred for 5 hours. The reaction mixture is washed with water, 2N citric acid, NaHCO3, and brine. The reaction mixture is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography on silica gel to give the desired product as a solid, m.p. 162°-188° C. (amorphous)

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05733905uspto-grants-1998_03