反应详情

温度

-20 °C

To a solution of 2-phenyl- pyrazolo-[1,5-a]-pyrimidine-5-carboxylic acid (120 mg), and triethylamine (0.091 ml) in tetrahydrofuran (10 ml), ethyl chlorocarbonate (0.053 ml) was added at −40° C. It was further added with a solution of 2-morpholinobenzylamine (115 mg) in tetrahydrofuran (2 ml), and thereafter heated to −20° C. The reaction solution was distilled under a reduced pressure, and then water was added thereto, extracted with chloroform, and the organic layer was dried with magnesium sulfate. After the reduced-pressure distillation of the solvent, the residue was purified by a silica gel column chromatography, and thereafter recrystallized from acetone-diisopropyl ether to yield N-(2-morpholinophenyl)methyl 2-phenyl-pyrazolo-[1,5-a]-pyrimidine-5-amide (142 mg, 69%). mp: 190-192° C.

1. distillationThe reaction solution was distilled under a reduced pressure
2. additionwater was added
3. extractionextracted with chloroform
4. dry with materialthe organic layer was dried with magnesium sulfate
5. distillationAfter the reduced-pressure distillation of the solvent
6. customthe residue was purified by a silica gel column chromatography
7. customrecrystallized from acetone-diisopropyl ether