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. 191980-54-8, name is 4-Iodo-1-trityl-1H-pyrazole, A new synthetic method of this compound is introduced below., COA of Formula: C22H17IN2
Example 95: Methyl (S)-{2,3,9-trimethyl-4-[4-(1H-pyrazol-4-yl)phenyl]-6H-thieno[3,2-f][1,2,4]triazolo[4,3-a][1,4]diazepin-6-yl}acetate To a mixture of the compound described in Starting Material Synthetic Example 1 (420 mg), tetrakistriphenylphosphine palladium”(58 mg) and 4-iodo-1-trityl-1H-pyrazole (654 mg) were added tetrahydrofuran (1.5 mL) and 2 M aqueous sodium carbonate solution (1.5 mL), and the mixture was stirred at 100C for 4 hr. After cooling, water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated. The residue was purified by column chromatography (chloroform:methanol=100:1) to give compound (729 mg). The obtained compound (729 mg) was dissolved in methanol (3 mL). Trifluoroacetic acid (154 muL) was added, and the mixture was stirred at room temperature for 2 days. After completion of the reaction, the mixture was neutralized with aqueous sodium hydroxide solution and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated. The residue was purified by column chromatography (chloroform:methanol=100:1) to give the title compound (162 mg) . 1H-NMR (400 MHz, DMSO-d6) delta: 2.67 (3H, s), 2.43 (3H, s), 2.62 (3H, s), 3.39-3.52 (2H, m), 3.68 (3H, s), 4.49 (1H, t, J = 7.2 Hz), 7.39 (2H, d, J = 8.2 Hz), 7.65 (2H, d, J = 8.2 Hz), 8.11 (2H, brs) MS (ESI) m/z: 447 (M+H)+.
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; Mitsubishi Tanabe Pharma Corporation; EP1887008; (2008); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics