Triethylamine → N-[4-(4H-Furo[2,3-e]pyrrolo[1,2-a][1,4]-diazepin-10(9H)-ylcarbonyl)phenyl]-2-methyl benzamide

HRID 1420002

Reaktionsgleichung

[CH3:1][C:2]1[CH:19]=[CH:18][CH:17]=[CH:16][C:3]=1[C:4]([NH:6][C:7]1[CH:15]=[CH:14][C:10]([C:11](Cl)=[O:12])=[CH:9][CH:8]=1)=[O:5].C(N(CC)CC)C.[O:27]1[C:31]2[NH:32][CH2:33][C:34]3[N:35]([CH:37]=[CH:38][CH:39]=3)[CH2:36][C:30]=2[CH:29]=[CH:28]1>C(Cl)Cl>[O:27]1[C:31]2[N:32]([C:11]([C:10]3[CH:14]=[CH:15][C:7]([NH:6][C:4](=[O:5])[C:3]4[CH:16]=[CH:17][CH:18]=[CH:19][C:2]=4[CH3:1])=[CH:8][CH:9]=3)=[O:12])[CH2:33][C:34]3[N:35]([CH:37]=[CH:38][CH:39]=3)[CH2:36][C:30]=2[CH:29]=[CH:28]1

Komponenten

Reaktionsbedingungen

Temperatur: 0 °C

Versuchsvorschrift

To a mixture of 1.1 mmol of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 10 ml of methylene chloride, cooled to 0° C. is added 1.5 mmol of triethylamine. To the mixture is added 1 mmol of 9,10-dihydro-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine and the mixture stirred at room temperature for 2 hours. The reaction mixture is concentrated in vacuo and the residue is dissolved in 100 ml of ethyl acetate and washed with water, 2N citric acid, aqueous NaHCO3 and brine. The solution is dried with Na2SO4 and the volatiles concentrated in vacuo to give a solid which is purified by flash chromatography to give the desired product.

Aufarbeitung

concentrationThe reaction mixture is concentrated in vacuo
dissolutionthe residue is dissolved in 100 ml of ethyl acetate
washwashed with water, 2N citric acid, aqueous NaHCO3 and brine
dry with materialThe solution is dried with Na2SO4
concentrationthe volatiles concentrated in vacuo
customto give a solid which
customis purified by flash chromatography

Quellen und Nachweise

ORD-Eintrag: ord-c593577e214a4a958805a8689975652a
Quelldatensatz: uspto-grants-1999_03
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05889001

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