反应详情

温度

60 °C

Crude 2-fluoro-5-(4-oxo-3,4,5,6,7,8-hexahydrophthalazin-1-ylmethyl)benzonitrile (10) (9.9 g, 34.9 mmol) was suspended in water (245 ml) and treated with sodium hydroxide (6.98 g, 174 mmol). The mixture was heated to 60° C. for 18 hours. The reaction was then cooled to 5° C. and concentrated sulfuric acid added dropwise until a precipitate formed (ca 10 ml, pH2). The suspension was stirred for 10 minutes at 5° C. and filtered. The solid isolated was washed with water (2×8 ml) and triturated with DCM (20 ml) before being dried. Single peak in LC-MS, (4.48 g, 98% purity) and was taken through to the next without any further purification; m/z (LC-MS, ESN), RT=1.96 mins (M−H 301.3).

1. temperatureThe reaction was then cooled to 5° C.
2. customformed (ca 10 ml, pH2)
3. filtrationfiltered
4. customThe solid isolated
5. washwas washed with water (2×8 ml)
6. customtriturated with DCM (20 ml)
7. custombefore being dried
8. customnext without any further purification