Electric Literature of 35179-98-7,Some common heterocyclic compound, 35179-98-7, name is Chloromethyl ethyl carbonate, molecular formula is C4H7ClO3, 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.
To a 100 ml of one-necked flask, 0.698g of material, 0.162g of potassium carbonate, 5 ml of N,N-dimethylacetamide were added in turn. The solution was stirred at room temperature for 20 minutes. Then 0.702g of chloromethyl ethyl carbonate was added and the mixture was reacted at 45-50C for 16 hours. After the reaction was completed, the mixture solution was filtered, and 30ml of water was added into the filtrate. The resulting mixture was extracted with 30ml of ethyl acetate twice. The organic phase was dried and concentrated to give 1.854g of oil, which was directly used in the next reaction without purification. 10ml of dioxane and 5ml of 4mol/L HCl were added and the resulting mixture was reacted at room temperature for 16 hours. The reaction was stopped and the solution was adjusted to pH 6-7 using aqueous sodium bicarbonate solution. The solution went turbid, and was extracted with ethyl acetate. The organic phase was washed with saturated brine, dried, concentrated to give 0.420g of 2-butyl-4-chloro-1-[2′-(1H-tetrazol-5-yl)1,1′-biphenyl-methyl] imidazole-5- carboxylic acid, 1-[(ethoxycarbonyl)oxy] methyl ester. 1H-NMR (CDCl3) delta H (ppm) 0.92(t,3H,J=17.5), 1,23(t,3H,J=14.0), 1.37(m,2H,J=34.2), 1.73(m,2H,J=30.8), 2.69(t,2H,J=15.5), 4.13(q,2H,J=15.7), 5.58(s,2H), 5,89(s,2H), 6,99-7.61(8H), 8.16(d,1H,J=6.1) ESI(-): 539.1 Mp:164.5-160C
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Chloromethyl ethyl carbonate, its application will become more common.
Reference:
Patent; SHANGHAI ALLIST PHARMACEUTICAL., INC.; EP1988090; (2008); A1;,
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