Triethylamine → 10,11-dihydro-10-(4-nitro-3-methoxybenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

To a solution of 0.55 g of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 8 ml of methylene chloride is added 0.55 g of triethylamine followed by 0.97 g of 3-methoxy-4-nitrobenzoyl chloride. The reaction mixture is stirred at room temperature for 2 hours and then quenched with 10 ml of 1N NaOH. The methylene chloride layer is evaporated and the resulting suspension filtered. The precipitate is washed with 1N NaOH (2×5 ml), water (3×5 ml) and hexane (2×5 ml). The collected solid is dried in vacuo to give 1.13 g of off-white solid. MS (CI): 364(M+H).

1. customquenched with 10 ml of 1N NaOH
2. customThe methylene chloride layer is evaporated
3. filtrationthe resulting suspension filtered
4. washThe precipitate is washed with 1N NaOH (2×5 ml), water (3×5 ml) and hexane (2×5 ml)
5. customThe collected solid is dried in vacuo

ORD-Eintrag

ord-9c6ae98e5dae4e6bb743c1f1090f4112

Quelldatensatz

uspto-grants-1997_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05624923