反应详情

To a mixture of 0.420 g of 2,4,5,6-tetrahydro-2-methyl-6-(4-aminobenzoyl)pyrazolo[4,3-d][1]benzazepine and 275 μl of triethylamine in 6 ml of methylene chloride and 2 ml of dioxane is added a solution of 215 μl of 2-methylbenzoyl chloride in 1.5 ml of dioxane. The reactants are stirred under argon for 4.5 hours. The volatiles are evaporated in vacuo to a residue which is dissolved in methylene chloride and washed with 10% NaHCO3 and brine. The organic layer is treated with activated carbon, dried with MgSO4 and evaporated in vacuo to give 660 mg of a tan foam residue. The residue is purified by column chromatography on silica gel by elution with 30% ethyl acetate-methylene chloride to give 590 mg of the desired product as white crystalline solid, m.p. 246°-248° C.; HR FABMS: (M+H)=437.1972.

1. customThe volatiles are evaporated in vacuo to a residue which
2. dissolutionis dissolved in methylene chloride
3. washwashed with 10% NaHCO3 and brine
4. additionThe organic layer is treated with activated carbon
5. dry with materialdried with MgSO4
6. customevaporated in vacuo