Extracurricular laboratory: Synthetic route of 936-16-3

As the rapid development of chemical substances, we look forward to future research findings about 936-16-3

2,3-Dihydrobenzo[d]isothiazole 1,1-dioxide, cas is 936-16-3, it is a common heterocyclic compound, the isothiazole compound, its synthesis route is as follows.,936-16-3

To a solution of {1-(tert-butyl)-5-(4-piperidin-1-yl-phenyl)-1H-pyrazol-3-yl}methanol (54.9 mg, 0.175 mmol) in methylene chloride (1.5 mL) were added PPh3 (93.1 mg, 0.355 mmol) and CBr4 (121 mg, 0.365 mmol) at 0¡ã C., followed by stirring at the same temperature for one hour to give {1-(tert-butyl)-5-(4-piperidin-1-yl-phenyl)-1H-pyrazol-3-yl}methyl bromide. When the reaction was completed as measured by TLC(Hexane:EtOAc=2:1), 1,2-benzisothiazoline-1,1-dioxide (27.3 mg, 0.161 mmol) in N,N-dimethylformamide (1.5 mL) was added dropwise. At the same temperature, potassium carbonate (228 mg, 1.65 mmol) was added, and the resulting solution was stirred for a day. When the reaction was completed as measured by TLC (Hexane:EtOAc=2:1), water was added, after which extraction was carried out with ethyl acetate and brine. The organic layer thus formed was dried over anhydrous magnesium sulfate, and concentrated in vacuo. The concentrate was purified by column chromatography (Hexane:EtOAc=4:1?1:1) to afford the title compound (15.2 mg, 20percent, white solid). (0324) M.P. 150.4-165.2¡ã C.; (0325) 1H NMR (300 MHz, CDCl3) delta 7.89 (d, J=7.9 Hz, 1H), 7.64-7.52 (m, 2H), 7.40 (d, J=7.1 Hz, 1H), 7.30-7.17 (m, 2H), 6.29 (d, J=8.7 Hz, 2H), 6.22 (s, 1H), 4.52 (s, 2H), 4.46 (s, 2H), 3.26-3.23 (brs, 4H), 1.79-1.74 (brs, 4H), 1.67-1.63 (brs, 2H), 1.49 (s, 9H); (0326) 13C NMR (75 MHz, CDCl3) delta 151.9, 144.4, 143.3, 135.4, 134.3, 132.5, 131.1, 128.9, 124.5, 123.7, 121.4, 114.9, 109.0, 61.0, 50.0, 41.4, 31.2, 25.7, 24.3

As the rapid development of chemical substances, we look forward to future research findings about 936-16-3

Reference£º
Patent; KOREA INSTITUTE OF SCIENCE AND TECHNOLOGY; NAM, Ghil Soo; CHOI, Kyung Il; KIM, Jung Hyun; PAE, Ae Nim; HONG, Jin Ri; LEE, Jae Kyun; (30 pag.)US2015/329533; (2015); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com