Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, A new synthetic method of this compound is introduced below., Safety of 2,4-Difluorobenzene-1-sulfonyl chloride
General procedure: To 5-(5-(5-Aminopyridin-3-yl)thiophen-2-yl)-2-methyl- isoindolin-1-one (225 mg, 0.79 mmol) in dry pyridine (23 mL) under N2 at RT, was added dropwise, 2,4-difluorobenzenesulphonyl chloride (336 mg, 1.58 mmol) in CH2C12 (3 mL) over 5 mm. The suspension was heated to 45C under N2 for 4 h., at which point another portion of 2,4-difluorobenzenesulphonyl chloride (169 mg,0.79 minol) in CH2C12 (2 mL) was added. The whole mixture was left to stir for at 45C under N2 for 16 h., then the solvent removed under reduced pressure. The resulting residue was suspended in acetone (10 mL), 1 M HCI (20 mL) added, and the entire mixture stirred for 10 minutes. The solid was then collected by filtration, washed well with 1 M HC1 and water, dried, and purified by chromatography as described below.In cases where the bis-sulphonarnide was also formed, a second step was introduced where the crude product above was treated with a 1:1 mixture of 1 ,4-dioxane and 2 M NaOH. The crude suiphomamide resulting from subsequent acidification of the reaction mixture was isolated by filtration, washed well with wafer, and dried. Purification was carried out by flash column chromatography (2% MeOHJCH2C12 as eluant), giving the title compound(1) as a pale yellow solid (211 mg, 54%), mp (MeOH/CH2C12) 266-269C. ?H NMR [400 MHz, (CD3)2S0] oe 11.15 (br s, 1 H), 8.69 (d, J= 2.0 Hz, I H), 8.25 (d, J= 2.4 Hz, 1 H), 8.01 (dt, J 8.7, 6.3 Hz, 1 H), 7.95 (s, I H), 7.83 (dd, J= 8.0, 1.5 Hz, 1 H), 7.68-7.75(m, 3 H), 7.65 (d, J 3.9 Hz, 1 H), 7.58 (dt, J 8.9, 2.4 Hz, I H), 7.30 (dt, J 8.2, 2.0 Hz,I H), 4.52 (s, 2 H), 3:09 (s, 3 H). Anal. (C24H17F2N303S2) C, H, N.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; PETER MACCALLUM CANCER INSTITUTE; SPICER, Julie Ann; DENNY, William Alexander; MILLER, Christian Karl; O’CONNOR, Patrick David; HUTTUNEN, Kristiina; TRAPANI, Joseph A.; HILL, Geoff; ALEXANDER, Kylie; WO2014/28968; (2014); A1;,
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