反应详情

2-(5-(7-Chloro-1-methyl-3-(naphthalen-2-ylmethyl)-2-oxo-2,3-dihydro-1H-benzo[e][1,4]diazepin-5-yl)pyridin-2-ylamino)-2-oxoethyl acetate (20 mg, 0.04 mmol) was dissolved in methanol (0.5 mL) and water (0.1 mL), potassium carbonate was added and the mixture was stirred at ambient temperature for 45 minutes. The crude mixture as partitioned between ethyl acetate and water, the layers were separated, and the organic layer was dried with sodium sulfate, decanted, then concentrated in the presence of silica gel. Column chromatography eluting with a step gradient of 20-80% ethyl acetate in hexanes in 5% increments every 3 minutes provided N-(5-(7-chloro-1-methyl-3-(naphthalen-2-ylmethyl)-2-oxo-2,3-dihydro-1H-benzo[e][1,4]diazepin-5-yl)pyridin-2-yl)-2-hydroxyacetamide (8 mg, 43% yield). ESI m/z measured 521.1348 [M+H]+. calculated 521.1356.

1. customThe crude mixture as partitioned between ethyl acetate and water
2. customthe layers were separated
3. dry with materialthe organic layer was dried with sodium sulfate
4. customdecanted
5. concentrationconcentrated in the presence of silica gel
6. washColumn chromatography eluting with a step gradient of 20-80% ethyl acetate in hexanes in 5% increments every 3 minutes