The synthetic route of 87691-88-1 has been constantly updated, and we look forward to future research findings.
87691-88-1, 3-Piperazinobenzisothiazole hydrochloride is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
87691-88-1, A mixture of 6-(2-chloro-ethyi)-7-fluoro-4,4,8-trimethyl-3,4-dihydro-1H-quinolin-2-one (0.7499 g, 2.780 mmol), 3-piperazin-1-yl-benzo[d]isothiazole hydrochloride (0.7834 g, 3.063 mmol), potassium carbonate (0.8456 g, 6.118 mmol) and potassium iodine (0.0495 g, 0.298 mmol) were reacted in acetonitrile (7.0 mL) in a CEM MARS5 microwave reactor for 1 h at 150 C. The reaction was cooled to room temperature, diluted with H2O (70 mL) and extracted with dichloromethane (2 x 75 mL). The organic extracts were combined, dried over anhydrous sodium sulfate, filtered and the solvent removed under reduced pressure. The resulting solid was purified by MPLC (The solid was washed with H2O and hexanes. The resulting solid was purified by MPLC (silica gel, 100% CH2CI2 to 3% MeOH/CH2CI2 over 1 h then hold at 3% MeOH/CH2CI2) to give a mixture of the titled compound and the product of step C. This mixture was dissolved in dichloromethane and 4 M hydrogen chloride in dioxane was slowly added until the product precipitated. The titled compound (0.3137 g, 0.660 mmol, 53% over two steps) was isolated as a white solid. MS (APCI): (M+1, free base)+= 439.2. 1H NMR (400 MHz, CDCl3) delta 1.29 (s, 6 H), 2.12 (d, J=1.6 Hz, 3 H), 2.44 (s, 2 H), 3.19 (s, 4 H), 3.32 (s, 2 H), 3.59 (s, 2 H), 4.17 (m, 4 H), 7.12 (d, J=7.6 Hz, 1H), 7.38-7.45 (m, 2 H), 7.49-7.54 (m, 1H), 7.84 (t, J=8.8 Hz, 2 H), 13.2 (br s, 1H). Anal, calcd. for C24H27FN4OS*HCl*0.75 H2O*0.10 CH2CI2: 58.24; H, 6.02; N, 11.27; H2O, 2.72. Found: 57.84; H, 6.17; N, 10.98; H2O, 2.57.
The synthetic route of 87691-88-1 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; WARNER-LAMBERT COMPANY LLC; WO2004/26864; (2004); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com