反应详情

A mixture of 4-methyl-5,6-dihydro-4H-1,3a,6-triaza-as-indacene-8-carboxylic acid hydrobromide (25 mg), aniline (12 mg), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (23 mg), 1,4-dioxane (1.5 mL), and water (1.5 mL) is stirred at room temperature for 4 days. 0.5N sodium hydroxide solution (3 mL) is added and the mixture is extracted with dichloromethane (3×50 mL). The combined organic layers are washed with brine (1×10 mL), dried over magnesium sulfate and concentrated in vacuo. The residue is purified by preparative thin layer chromatography on silica gel, eluting with 5% methanol in dichloromethane, to give 4-methyl-5,6-dihydro-4H-1,3a,6-triaza-as-indacene-8-carboxylic acid phenyl amide, cream solid, 7 mg: LRMS calcd 292.34, found [M+H] 293.2.

1. extractionthe mixture is extracted with dichloromethane (3×50 mL)
2. washThe combined organic layers are washed with brine (1×10 mL)
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue is purified by preparative thin layer chromatography on silica gel
6. washeluting with 5% methanol in dichloromethane