A new synthetic route of 1065114-27-3

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, tert-Butyl 2,4-dichloro-8,9-dihydro-5H-pyrimido[4,5-d]azepine-7(6H)-carboxylate, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 1065114-27-3, name is tert-Butyl 2,4-dichloro-8,9-dihydro-5H-pyrimido[4,5-d]azepine-7(6H)-carboxylate, belongs to amides-buliding-blocks compound, 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 1065114-27-3, SDS of cas: 1065114-27-3

2,4-Dichloro-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine hydrochloride (4.79 g, 18.4 mmol) was suspended in dichloromethane (50 mL), and the suspension was mixed with di-tert-butyl dicarbonate (6.0 g) and triethylamine (7.7 mL), followed by stirring at room temperature for thirty minutes. The reaction mixture was mixed with a saturated aqueous sodium bicarbonate solution, was stirred for a while and was separated. The organic layer was washed with brine and was dried over anhydrous sodium sulfate. After distilling off the solvent, the whole quantity of the residue was dissolved in tetrahydrofuran (50 mL), and the solution was mixed with 2 , 4-dichlorobenzylamine (4.2 mL) and triethylamine (11.5 mL), followed by stirring at 40C for 21 . 5 hours. The reaction mixture was diluted with water and was extracted with ethyl acetate. The organic layer was washed with brine, was dried over anhydrous sodium sulfate, and the solvent was distilled off. The residue was mixed with ethyl acetate for crystallization. The precipitated crystals were collected by filtration, were dried and thereby yielded tert-butyl 2-chloro-4-(2,4-dichlorobenzylamino)-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine-7-carboxylate (4.27 g). After concentrating the filtrate, the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1) and thereby yielded the target compound (0.76 g, 5.03 g in total with the above-mentioned crystals, in a yield of 60%).

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, tert-Butyl 2,4-dichloro-8,9-dihydro-5H-pyrimido[4,5-d]azepine-7(6H)-carboxylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; KYOWA HAKKO KOGYO CO., LTD.; EP1552842; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics