반응 #1507169

반응 방정식

10,11-dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

o-tolyl isocyanate

→

desired product

수율 56.1%

10,11-Dihydro-10-[4-[[[(2-methylphenyl]amino]carbonyl]amino]benzoyl]-5H-pyrrolo[2,1-c][1,4]benzodiazepine

수율 56.1%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도is heated
2. 2
   온도at reflux under argon for 24 hours
3. 3
   기타The volatiles are evaporated in vacuo to a residue which
4. 4
   workup.DISSOLUTIONis dissolved in methylene chloride
5. 5
   workup.ADDITIONHexane is added to the filtrate at the boil

실험 절차

A mixture of 0.93 g 10,11-dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine and 0.37 g of o-tolyl isocyanate in 50 ml of tetrahydrofuran is heated at reflux under argon for 24 hours. The volatiles are evaporated in vacuo to a residue which is dissolved in methylene chloride and passed through a pad of hydrous magnesium silicate. Hexane is added to the filtrate at the boil to give 0.68 g of the desired product as crystals, m.p. 155°-158° C.

출처