반응 #2323982

반응 방정식

tert-butyl 4-(4-{[(Z)-(6-iodo-1,3-dioxo-2,3-dihydroisoquinolin-4(1H)-ylidene)methyl]amino}phenyl)piperazine-1-carboxylate

phosphoric acid

→

title compound

수율 24.2%

(4Z)-6-Iodo-4-{[(4-piperazin-1-ylphenyl)amino]methylene}isoquinoline-1,3(2H,4H)-dione

수율 24.2%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타After evaporating to dryness
2. 2
   기타the residue is partitioned between methylene chloride and saturated sodium bicarbonate
3. 3
   세척The organic layer is washed with water
4. 4
   기타dried
5. 5
   기타evaporated

실험 절차

A N,N-dimethylformamide mixture (0.6 mL) of tert-butyl 4-(4-{[(Z)-(6-iodo-1,3-dioxo-2,3-dihydroisoquinolin-4(1H)-ylidene)methyl]amino}phenyl)piperazine-1-carboxylate (50 mg, 0.087 mmol) and concentrated phosphoric acid (0.6 mL) is heated at 60 C for 2 h. After evaporating to dryness, the residue is partitioned between methylene chloride and saturated sodium bicarbonate. The organic layer is washed with water, dried, and evaporated to yield 10 mg (24%) of the title compound as an orange solid. MS (ESI) m/z 475.2 (M+H)+1

출처