Dichloromethane → HCID 86641349, compound

Participants

Reaction Conditions

Reaction Steps

Mesyl chloride (5 μl) was added dropwise to a mixture composed of tert-butyl {8-(2-hydroxyethyl)-2-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-4-yl}carbamate of Example 134 (25 mg), dehydrated dichloromethane (0.5 ml) and triethylamine (15 μl) under ice-cooling, and the mixture was stirred at 0° C. for 10 minutes. After confirming that the raw material disappeared, the solvent in the reaction mixture was evaporated by spraying. Dioxane (0.2 ml) and morpholine (44 μl) as an amine were added to the residue, and the mixture was stirred at 60° C. for six hours. The reaction mixture was concentrated under reduced pressure, and a 0.5 N sodium hydroxide solution was added to the resulting residue, followed by extraction with ethyl acetate. The organic layer was concentrated, and the resulting residue was purified by NH silica gel column chromatography (hexane-ethyl acetate) to obtain the title compound (17 mg, 60%) as an oil.

Provenance & Evidence