Category: 101066-61-9

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. 101066-61-9, name is 2-Chloroisonicotinaldehyde. A new synthetic method of this compound is introduced below., HPLC of Formula: C6H4ClNO

To a solution of 2-chloroisonicotinaidehyde (230 mg, 1.60 mmoi) in DCM (3 mL) was added DAST (773 mg, 4,80 rnrnol) at 0C under N2 and the mixture stirred at 0C for lh. Saturated aq. NaHCO3 was added and the mixture extracted with EtOAc (30 rnL x 3). The combined organic layers were dried over MgSO4, filtered, the filtrate concentrated in vacuo and the crude product purified by chromatography on silica (50% EtOAc in petroleum ether) to givethe title compound as an oil. LRMS mlz (M+H) 164.1 found, 164.1 required.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 101066-61-9, 2-Chloroisonicotinaldehyde.

Reference:
Patent; MERCK SHARP & DOHME CORP.; KUDUK, Scott D.; LIVERTON, Nigel; LUO, Yunfu; SKUDLAREK, Jason; (79 pag.)WO2016/95204; (2016); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 101066-61-9, 2-Chloroisonicotinaldehyde, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, category: pyridine-derivatives, blongs to pyridine-derivatives compound. category: pyridine-derivatives

A slurry of 2-chloro-4-formylpyridine (1.49 Kg, 10.5 mole, 1.05 equiv), 2-aminothiazole (1.27 Kg, 10.0 mole, 1.0 equiv), K3PO4 (2.34 Kg, 11.0 mole, 1.1 equiv) in toluene (20 L) is degassed by two vacuum/nitrogen cycles. Pd2(dba)3 (114.5 g, 0.125 mmol, 2.5mol % Pd) and Xantphos (159 g, 0.275 mole, 2.75mol %) are then added and the mixture is degassed by one vacuum/nitrogen cycle followed by bubbling nitrogen through the slurry for 10 minutes. The mixture is heated to 60 C. and degassed water (90 mL, 5.0 mole, 0.5 equiv) was added over 5 minutes. The mixture is then heated to 90 C. and aged for 8 h. [0227] It is cooled to rt and filtered. The filter cake is washed with toluene (20 L) until very little DBA is observed in the wash. DMAc (24 L) is added to the filter cake to dissolve the product. The insoluble is filtered off and washed with more DMAc (6 L). The filtrate is acidified with concentrate HCl (110 mL) to pH 2.7. Water (3 L) is added and the mixture is concentrated at 40-50 C. under vacuum to remove most of the residual toluene by azeotropic distillation. More water (3 X 1L) is added as the distillation progress. [0228] The mixture is seeded and then water (13 L) is added at a rate of about 1.3 L/h. The product is filtered and washed with 5/4 DMAc/water (4.0 L X 2), water (4.0 L), acetone (4 L X 2), and then oven dried at 40 C. under vacuum (100 mmHg) with nitrogen sweep to give the product.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,101066-61-9, 2-Chloroisonicotinaldehyde, and friends who are interested can also refer to it.

Reference:
Patent; Zhao, Matthew M.; Bilodeau, Mark T.; US2004/23980; (2004); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem