In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 109-85-3 as follows. SDS of cas: 109-85-3
A) Chloro(N-(2-methoxyethyl))acetamide, (1) In a three-necked 2L round bottom flask fitted with two 500mL addition funnels, containing 56.4g (39.8mL, 0.50mole) chloroacetyl chloride in 400mL dichloromethane and 20g (0.50mole) sodium hydroxide in 400mL water, respectively, and a water-cooled condenser, was placed 35.7g (41.3mL, 0.48mole) 2-methoxyethylamine, 100mL water, 100mL dichloro-methane. The reaction vessel was cooled to 0 C. by a salt-ice bath. The organic and aqueous solutions were allowed to add slowly, -0.25mL per minute, to the reaction mixture. During the addition the pH of the water phase of the reaction was monitored and the rate of addition of the alkali solution adjusted so as to maintain pH=12. When the addition was complete, the mixture was allowed to warm to room temperature and stir overnight. The organic layer was removed by siphon and dried with magnesium sulfate for four hours. The mixture was filtered through #4 filter paper on a large Buchner funnel and the sulfate washed with 2*100mL fresh dichloromethane. The combined filtrates were then placed in 2L round bottomed flask and the mixture distilled at torr. Fractions collected from 55 C. to 60 C. were combined and analyzed by NMR. Yield 31.lg (43% based on starting 2-methoxyethylamine). TLC (silica on glass, 2% methanol in dichloromethane) R67 =0.40. 1 H(delta, CDCl3) 3.28(s,3H), 3.40{m,4H}, 3.97{s,2H}, 6.92{br, IH}. 13 C{1 H}{delta, CDCl2 }39.27, 42.32, 58.60, 70.54, 166.22.
According to the analysis of related databases, 109-85-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Mallinckrodt Medical, Inc.; US5138040; (1992); A;,
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