Related Products of 20485-43-2,Some common heterocyclic compound, 20485-43-2, name is 1-Methyl-1H-imidazole-2-carboxylic acid, molecular formula is C5H6N2O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
General procedure: Reaction monitoring. To check the progress of the reaction, some resin beadswere taken, mixed with 30 muL of 95% TFA solution and shaken for a fewseconds, while the beads turn red. The supernatant solution was removed andmixed 1:1 with H2O. 1 muL of the aqueous solution was mixed with 1 muL of DHBmatrix on the target, dried and the mass spectrum was measured by MALDI-ToF-MS. If necessary, the deprotection was repeated.Fmoc deprotection. The amino protecting group Fmoc was cleaved after eachcoupling step to allow the coupling of the next amino acid. For this, the resinwas swollen in DMF and then suspended three times for 15 minutes in a 20%piperidine solution in DMF. The resin was filtered off and washed twice withCH2Cl2, DMF and again CH2Cl2.Coupling reactions. The resin was swollen in DMF. The amino acid (3 equiv)was dissolved in DMF containing DIPEA (9 equiv) and the coupling reagent(HBTU or PyBOP, 3 equiv) was added for pre-activation. After 5 minutes thesolution was added to the resin, and the suspension was mixed for 1.5 hours byshaking. The resin was then filtered off with suction and washed twice withCH2Cl2, DMF and again CH2Cl2. The completeness of the reaction was checkedwith MALDI-ToF-MS. If necessary, the coupling reaction was repeated.Cleavage from the resin. After swelling in CH2Cl2, the acid-labile 2 chlorotritylresin containing the polyamide was mixed with a 2.5% solution ofS7CH2Cl2/TFA/TIS 95:2.5:2.5 (v/v/v), mixed for 5 minutes and filtered off. This wasrepeated until the discoloration of the filtrate was complete. The combinedfiltrates were evaporated and the oily residue was treated with a mixtureH2O:MeCN and lyophilized.
The synthetic route of 20485-43-2 has been constantly updated, and we look forward to future research findings.