Day: September 13, 2021

Synthetic Route of 101990-69-6, Adding some certain compound to certain chemical reactions, such as: 101990-69-6, name is 2,6-Dichloropyridine-4-methanol,molecular formula is C6H5Cl2NO, 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 101990-69-6.

a) 4-(tert-Butyl-dimethyl-silanyloxymethyl)-2,6-dichloro-pyridine; A solution of 2,6-dichloropyridine-4-methanol (150 mg, 0.84 mmol), tert-butyl-chloro-dimethyl-silane (152 mg, 1.01 mmol) and imidazol (143 mg, 2.01 mmol) in 1 mL of N,N-dimethylformamide was stirred overnight at. The reaction mixture was concentrated in the rotatory evaporator, water was added and the slurry extracted with ethyl acetate. Chromatography on amino-modified silica gel (Merck HPTLC Silica Gel 60 NH2F254S) using heptane/ethylacetate (gradient 0 to 50% ethyl acetate) gave the pure title compound as a colorless solid (160 mg, 65%). MS ISP (m/e): 292.1 & 294.0 (100 & 97) [(M+H)+]. 1H NMR (CDCl3, 300 MHz): delta (ppm)=7.21 (s, 2H), 4.70 (s, 2H), 0.95 (s, 9H), 0.12 (6H).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 101990-69-6, 2,6-Dichloropyridine-4-methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Baumann, Karlheinz; Flohr, Alexander; Goetschi, Erwin; Jacobsen, Helmut; Jolidon, Synese; Luebbers, Thomas; US2009/215759; (2009); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 89-00-9 , The common heterocyclic compound, 89-00-9, name is Pyridine-2,3-dicarboxylic acid, molecular formula is C7H5NO4, its 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.

Pyridine-2,3-dicarboxylic acid (8.40 g, 50.30 mmol, 1 eq) was suspended in acetic anhydride (11.0 mL, 116.50 mmol, 2.3 eq) and the mixture was heated at 120 C, distilling 9.5 mL of acetic acid. After cooling at 100 C the acetamide (6.70 g, 113.60 mmol, 2.2 eq) was added portionwise in 5 min. The reaction was then heated at reflux for 2.5 h. After cooling at room temperature, the precipitate was filtered off and washed with water (2 * 12 mL) to give the desired product as grey solid after crystallization with EtOH/H2O 95:5 (3.46 g, 47%). Mp. 230-231 C. 1H NMR (300 MHz, DMSO-d6) delta 11.63 (br s, NH), 8.93 (d, J = 4.9 Hz, 1-H), 8.22 (d, J = 7.7 Hz, 1-H), 7.74 (dd, J = 7.6/4.9 Hz, 1-H). IR (KBr) 3483, 3189, 3100, 1735, 1704 cm-1.

The synthetic route of 89-00-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Galli, Ubaldina; Mesenzani, Ornella; Coppo, Camilla; Sorba, Giovanni; Canonico, Pier Luigi; Tron, Gian Cesare; Genazzani, Armando A.; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 58 – 66,9;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem