The synthetic route of 250285-32-6 has been constantly updated, and we look forward to future research findings.
With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.250285-32-6,1,3-Bis(2,6-diisopropylphenyl)imidazolium chloride,as a common compound, the synthetic route is as follows.
Finely powdered PdCl2 (177 mg, 1.00 mmol) was suspended in CH3CN (5 mL), and N- benzyldimethylamine (160 muL, 143 mg, 1.05 mmol) were added. The solution was heated to 8O0C with stirring a until clear, orange solution was formed (approx. 20 min). Finely powdered K2CO3 (691 mg, 5.00 mmol) was added and the stirring was continued until palladacycle formation was complete, as indicated by the formation of a canary yellow solution (5-10 min) . IPr-HCl (467 mg, 1.10 mmol) was added and the mixture was stirred at 8O0C over 18h. The reaction mixture was filtered and evaporated. The resulting product was purified by column chromatography. Upon application of the product to a pad of silica gel (2.5 x 8 cm) pre-equilibrated with CH2Cl2, CH2Cl2 (100 mL) was used to elute impurities. The pure NHC-palladacycles were eluted with CH2Cl2-ethylacetate (3:1, vol/vol, 150 mL), and the solvents were evaporated. The products were triturated with hexanes (25 mL). After drying in high vacuum, IPr- Pd(dmba)Cl (543 mg, 82%) was obtained as beige solid. 1H NMR (CDCl3, 400 MHz) delta: 7.40 (t, J= 7.6 Hz, 2H), 7.30 (d, J= 7.6 Hz, 2H); 7.21 (s, 2H), 6.82-6.70 (m, 3H), 6.53 (d, J = 7.6 Hz, IH), 3.46 (s, 2H), 3.37 (m, 2H), 3.15 (m, 2H)5 2.39 (s, 6H)5 1.49 (d, J= 6.8 Hz, 6H), 1.18 (d, J= 6.8 Hz, 6H), 1.02 (d, J= 6.8 Hz, 6H), 0.81 (d, J= 6.4 Hz, 6H). 13C NMR (CDCl3, 100 MHz) delta: 177.5, 150.5, 147.8, 147.8, 144.7, 136.2, 136.1, 129.7, 125.4, 124.6, 124.0, 123.8, 122.6, 121.5, 72.6, 49.8, 29.0, 28.3, 26.4, 26.2, 23.2, 23.2. Anal, calcd for C36H48ClN3Pd (665.67): C, 65.05; H, 7.28; N, 6.32. Found: C, 65.14; H, 7.41; N, 6.53.
The synthetic route of 250285-32-6 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; AGENCY FOR SCIENCE, TECHNOLOGY AND RESEARCH; WO2008/156451; (2008); A1;,
Chiral Catalysts
Chiral catalysts – SlideShare