95-15-8, Thianaphthene is a benzothiophene compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,95-15-8
Step C: Synthesis of Compound 6; The compound 2 (13.420 g, 100.0 mmol) and a stir bar were placed in a 300-ml three-neck flask and nitrogen replacement was carried out in the reaction vessel. Next, anhydrous Et2O (200 ml) was added and the reaction vessel was cooled to -15 C. Then, n-BuLi (2.44M hexane solution, 40.98 ml, 110.0 mmol) was added and the mixture was stirred at -15 C. for 30 minutes. Next, elemental sulfur (7.697 g, 240.0 mmol) was slowly added and the mixture was stirred at a room temperature for 11 hours. Water was poured into the reaction mixture and hydrochloric acid was added to adjust the pH of the solution to 1.0. After being extracted with CH2Cl2, the organic layer was dried over anhydrous magnesium sulfate and filtered. Then, the solvent was removed by a rotary evaporator. The reaction mixture obtained was dissolved into 100 ml of tetrahydrofuran (THF). After slowly adding sodium tetrahydroborate (3.782 g, 100.0 mmol) at a room temperature, the mixture was stirred for 1 hour as it was. Next, water was poured into the reaction solution and hydrochloric acid was added to adjust the pH of the solution to 1.0. After being extracted with Et2O, an aqueous solution of 5.0M sodium hydroxide was added to the organic phase to make the mixture basic. Then, the aqueous phase was separated and hydrochloric acid was added to the aqueous phase to adjust its pH to 1.0. After being extracted with CH2Cl2, the organic layer was dried over anhydrous magnesium sulfate and filtered. Then, the solvent was removed by the rotary evaporator. Through silica gel column chromatographly using hexane as a developing solvent, the compound 6 (9.156 g, 55.07 mmol, 55%) was separated and purified as a white solid. Structural data of the compound were as follows: 1H NMR (400 MHz, CDCl3) delta 3.67 (d, 1H, J=1.0 Hz, SH), 7.26 (brs, 1H, ArH), 7.29 (dd, 1H, J=7.5, 1.7 Hz, ArH), 7.30 (dd, 1H, J=7.2, 1.4 Hz, ArH), 7.65 (dd, 1H, J=6.9, 2.0 Hz, ArH), 7.70 (dd, 1H, J=7.0, 1.8 Hz, ArH).
The synthetic route of 95-15-8 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; SEIKO EPSON CORPORATION; US2008/76935; (2008); A1;,
Benzothiophene – Wikipedia
Benzothiophene | C8H6S – PubChem