反应详情

A solution of 1-benzyl-5′-oxo-2′-(4-phenoxyphenyl)-5′,6′-dihydro-4′H-spiro[piperidine-4,7′-pyrazolo[1,5-a]pyrimidine]-3′-carbonitrile (500 mg, 1.02 mmol) in H3PO4 (5 mL) was heated to 130° C. for 1 hr. The mixture was poured to water (20 mL) and extracted with EA (20 mL×3). The combined organic layers were dried over Na2SO4, concentrated and purified by chromatography column on silica gel using 5% of MeOH in DCM as eluant to afford the product (180 mg, 34.8%) as a yellow solid. MS (ESI, m/e) [M+1]+ 507.9.

1. extractionextracted with EA (20 mL×3)
2. dry with materialThe combined organic layers were dried over Na2SO4
3. concentrationconcentrated
4. custompurified by chromatography column on silica gel using 5% of MeOH in DCM as eluant