反应详情

温度

105 °C

A mixture of 3-(1-hydroxyphthalazin-6-yl)-4-methylbenzoic acid (1.08 g, 3.85 mmol) and phosphorus oxychloride (25.0 mL, 268 mmol) was heated to 105° C. for 3 h. After cooling to RT, the solvents were removed in vacuo. The residue was re-dissolved in CH2Cl2 and treated carefully with cyclopropylamine (1.36 mL, 19.3 mmol) at RT. The mixture was diluted with sat aq. NaHCO3 and H2O and extracted with CH2Cl2 (4×). The combined organics were dried over Na2SO4, filtered and concentrated. The residue was purified using column chromatography (MeOH/CH2Cl2=0→3%). Found MS (ESI, pos. ion) m/z: 338 (M+1).

1. temperatureAfter cooling to RT
2. customthe solvents were removed in vacuo
3. dissolutionThe residue was re-dissolved in CH2Cl2
4. extractionextracted with CH2Cl2 (4×)
5. dry with materialThe combined organics were dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified