Ethyl Acetate → 1(2H)-Phthalazinone

Temperature

0 °C

To 4-(3-(4-(2-((2,4-dichlorophenyl)thio)-2-methylpropanoyl)piperazine-1-carbonyl)-4-fluorobenzyl)phthalazin-1(2H)-one (2.5 g, 15 mmol) in MeOH (25 mL) was added dropwise a solution of Oxone (9.98 g, 30 mmol) in water (25 mL) at 0° C. after addition reaction mixture stirred at 0° C. for 4 h. The progress of reaction was checked by TLC using mobile phase 50% ethyl acetate in pet ether. The reaction mixture was evaporated on a rotatory evaporator under reduced pressure to afford the semisolid off-white compound. The suspension was diluted with water and then extracted with ethyl acetate. The organic layer was washed with brine solution, dried over anhydrous Na2SO4 and solvents were evaporated on a rotatory evaporator under reduced pressure to afford 4-(3-(4-(2-(2,4-dichlorophenyl)sulfinyl)-2-methylpropanoyl)piperazine-1-carbonyl)-4-fluorobenzyl)phthalazin-1(2H)-one (39) as off-white crystals compound (1.4 g, 32%)

1. additionafter addition reaction mixture
2. customThe progress of reaction
3. customThe reaction mixture was evaporated on a rotatory evaporator under reduced pressure
4. customto afford the semisolid off-white compound
5. extractionextracted with ethyl acetate
6. washThe organic layer was washed with brine solution
7. dry with materialdried over anhydrous Na2SO4 and solvents
8. customwere evaporated on a rotatory evaporator under reduced pressure

ORD record

ord-9f401877cc83414782c5870729857cf6

Source dataset

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08871765B2