Analyzing the synthesis route of 770-08-1

The synthetic route of 770-08-1 has been constantly updated, and we look forward to future research findings.

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 770-08-1, name is 5-Ethylpicolinic acid, the common compound, a new synthetic route is introduced below. Computed Properties of C8H9NO2

Example IV; Preparation of [1-(6-trichloromethylpyridin-3-yl)ethyl](methyl)-oxido-lambda4-sulfanylidenecyanamide (5); A mixture of 5-ethylpyridine-2-carboxylic acid (1.98 g, 13 mmol), phenyl-phosphonic dichloride (2.8 g, 14.3 mmol), phosphorus pentachloride (7.7 g, 32 mmol) was stirred and slowly heated. Once a clear yellow liquid was formed, the mixture was heated to reflux overnight. After cooling, the volatiles were removed under reduced pressure. The residue was carefully poured into saturated sodium carbonate aqueous solution cooled in an ice-water bath. The aqueous phase was then extracted with CH2Cl2 two times. The combined organic layer was washed with brine, dried over anhydrous Na2SO4, filtered, concentrated, and partially purified on silica gel eluted with 10 percent EtOAc in hexane to give 2.7 g of crude product containing both 5-ethyl-2-(trichloromethyl)pyridine and 5-(1-chloro-ethyl)-2-(trichloromethyl)pyridine in an approximate 3:1 ratio (GC data, masses calcd for C8H8Cl3N and C8H7Cl4N [M]+223 and 257 respectively. Found 223 and 257 respectively).; A mixture of the above-mentioned crude product (2.6 g) in carbon tetrachloride (100 mL) was then treated with 80 percent of N-bromosuccinimide (1.9 g, 11 mmol) and benzoylperoxide (0.66 g, 0.275 mmol) and then refluxed overnight. The solid was filtered off, the filtrate concentrated and the resulting residue purified on silica gel using 4 percent EtOAc in hexane to give 1.0 g of the desired product 5-(1-bromoethyl)-2-(trichloromethyl)pyridine (A) as a yellow solid. The combined yield for the two steps was 25 percent. GC-MS: mass calcd for C8H7BrCl3N [M-I-Cl]+266. Found 266.

The synthetic route of 770-08-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dow AgroSciences, LLC; US2010/168177; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem