652-39-1, 4-Fluoroisobenzofuran-1,3-dione is a benzofuran compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
Step 1: 5-fluoro-2-methyl-2,3-dihydrophthalazine-1,4-dione and 8-fluoro-2-methyl-2,3-dihydrophthalazine-1,4-dione A mixture of 4-fluoroisobenzofuran-1,3-dione (5.0 g, 30.10 mmol) and methylhydrazine (40percent aq., 3.5 g, 30.10 mmol) in ethanol (100 mL) was heated at reflux for 15 h, at which time LCMS indicated that the reaction had gone to completion. The mixture was concentrated under reduced pressure to give the mixture of title compounds (3.5 g, 60percent yield) (2 : 1 ratio of regioisomers) as a yellow solid. This crude material was used in the next step without further purification. LCMS M/Z (M+H) 195. Step 2: 4-chloro-5-fluoro-2-methylphthalazin-1(2H)-one and 4-chloro-8-fluoro-2-methylphthalazin-1(2H)-one A mixture of 5 or 8-fluoro-2-methyl-2,3-dihydrophthalazine-1,4-dione (3.5 g, 18.03 mmol) in POCl3 (50 mL) was heated at reflux for 15 h, at which time LCMS indicated that the reaction had gone to completion. The mixture was concentrated under reduced pressure, the residue was quenched by addition a saturated aqueous solution of NaHCO3 (100 mL), and then extracted with ethyl acetate (3 x 100 mL). The combined organic extracts were dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by silica gel chromatography (petroleum ether : Ethyl acetate = 5: 1) to give the title compounds (1.2 g, 31percent yield) (2 : 1 ratio of regioisomers) as a white solid. LCMS M/Z (M+H) 213.
The synthetic route of 652-39-1 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; GENENTECH, INC.; CONSTELLATION PHARMACEUTICALS, INC.; ALBRECHT, Brian, K.; COTE, Alexandre; CRAWFORD, Terry; DUPLESSIS, Martin; GOOD, Andrew, Charles; LEBLANC, Yves; MAGNUSON, Steven; NASVESCHUK, Christopher, G.; PASTOR, Richard; ROMERO, F. Anthony; TAYLOR, Alexander, M.; (179 pag.)WO2016/36954; (2016); A1;,
Benzofuran – Wikipedia
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