Analyzing the synthesis route of Ethyl 2-hydroxyacetate

Statistics shows that 623-50-7 is playing an increasingly important role. we look forward to future research findings about Ethyl 2-hydroxyacetate.

Application of 623-50-7, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.623-50-7, name is Ethyl 2-hydroxyacetate, molecular formula is C4H8O3, molecular weight is 104.1045, as common compound, the synthetic route is as follows.

Example 34[0196] Preparation of allyloxy-acetic acid ethyl ester. EMI61.2[0197] A round-bottom flask was charged with NaH (1.76 g, 44 mmol, 60% dispersion in mineral oil) and flushed with argon. Hexane (10 ml x 2) was added and decanted. DMF (10 ml) was added into the flask and the resulting solution was cooled to 0 C. Ethyl glycolate (4.16 g, 40.0 mmol) was added over 10 min. The solution was allowed to gradually warm to 25 C and was maintained at that temperature for 2 h. The solution was cooled to 0 C and allyl bromide (5. 32 g, 44.0 mmol) was added over 10 min. The solution was allowed to gradually warm to 25 C and stirred at that temperature for 2h. Aqueous solutionNH4Cl(10 ml) was added to the reaction and the mixture was diluted with EtOAc (60 ml). The organic layer was separated and washed withH20 (20 ml x 2), dried overNa2S04 and concentratedin vacuo. The crude product was purified by distillation under reduced pressure. [0198] Yield = 4.29 g, 75%; colorless liquid; bp = 38-39 C, 2 mmHg. IR (neat): 1985,1756, 1724,1203, 1130 cm-l. IH NMR (CDC13, 400 MHz): 6 5.90-5. 70 (m, 1H), 5.25-5. 00 (m, 2H), 4.10-4. 20 (m, 2H), 3.92-4. 05 (m, 4H), 1.21 (t, J = 7Hz, 3H). 13C NMR (CDCl3, 100 MHz): 8 170.09 (C), 133.62 (CH), 117.78 (CH2), 72.10 (CH2), 66.99 (CH2), 60.53 (CH2), 13. 94 (CH3). MS (m/z, relative intensity): 144 (M+, 14), 115 (22), 103 (100), 83 (85); HRMS: calculated for C7HI203 (M+): 144.0786 ; found 144.0783.

Statistics shows that 623-50-7 is playing an increasingly important role. we look forward to future research findings about Ethyl 2-hydroxyacetate.

Reference:
Patent; AUSPEX PHARMACEUTICALS, INC.; WO2005/49582; (2005); A1;,
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