Triethylamine → N-[4-[(6,7-Dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-5-yl)carbonyl]-3-chlorophenyl]-2,4-dichlorobenzamide

To a mixture of 0.10 g of 6,7-dihydro-5-(4-amino-2-chlorobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine and 0.06 g of triethylamine in 6 ml of dichloromethane is added 0.10 g of 2,4-dichlorobenzoyl chloride in 0.5 ml of dichloromethane. The mixture is stirred at room temperature for 2 hours and 2 ml of 1N NaOH is added. The volatiles are removed under vacuum and to the residue is added 2 ml of tetrahydrofuran and 1 ml of methanol. The mixture is stirred at room temperature for 2 hours and the volatiles removed. To the residue is added 2 ml of 1N NaOH and 5 ml of H2O. The mixture is extracted with ethyl acetate and the extract washed with brine and dried (Na2SO4). The solvent is removed and the solid triturated with diethyl ether-hexane to give 0.15 g of white solid, Mass Spectrum (CI): 510(M+H, Cl35).

1. customThe volatiles are removed under vacuum and to the residue
2. additionis added 2 ml of tetrahydrofuran and 1 ml of methanol
3. stirringThe mixture is stirred at room temperature for 2 hours
4. customthe volatiles removed
5. additionTo the residue is added 2 ml of 1N NaOH and 5 ml of H2O
6. extractionThe mixture is extracted with ethyl acetate
7. washthe extract washed with brine
8. dry with materialdried (Na2SO4)
9. customThe solvent is removed
10. customthe solid triturated with diethyl ether-hexane

ORDレコード

ord-11dd793ef6d44dfb954c77ff0c37036a

出典データセット

uspto-grants-1998_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05733905