Application of 6065-82-3, A common heterocyclic compound, 6065-82-3, name is Ethyl diethoxyacetate, molecular formula is C8H16O4, 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.
Example 6An ethyl ester compound according to formula Illb1 wherein Q = OEt (10,11-dihydro- 5H-benzo[e]pyrido[2,3-b]azepine-10-carboxylic acid ethyl ester ) was prepared as described below.A mixture of 2-amino-3-benzylpyridine (2.1 g, 11.4 mmol) and ethyl 2,2-diethoxyacetate (3.8 g, 21.6 mmol, 1.9 eq.) in a 250 ml round-bottomed flask was treated at room temperature with concentrated sulphuric acid (10 ml) by quick addition while stirring. A vigorous exothermic reaction took place. After stirring for 30 minutes the dark mixture was poured on ice water (100 ml). Concentrated ammonia (25% aq.; 25 ml) was added to basify the mixture. Extraction with ethyl acetate (2 x 50 ml). The combined organic layers were dried with Na2SO4. Evaporation under vacuum gave 10,11-dihydro-5H- benzo[e]pyrido[2,3-b]azepine-10-carboxylic acid ethyl ester as a dark yellow oil (2.4 g, 8.9 mmol) in 79% c.y. An analytically pure sample can be obtained by chromatography on silica gel. Rf = 0.3 (EtOAc/n-heptane = 1 :1 ). Mass analysis: M+1 = 269 major peak. 1H-NMR (CDCI3) delta (ppm) 1.28 3H, d, J = 7.2 Hz, CH3; 3.80 1 H, d, J = 15.5 Hz, CHH; 4.18 1 H, d, J = 15.5 Hz, CHH; 4.32 2H, q, J = 7.2 Hz, OCH2; 5.54 1 H, d, J = 5.1 Hz;
The synthetic route of 6065-82-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; N.V. ORGANON; SEERDEN, Johannes Paulus Gerardus; WO2008/125577; (2008); A1;,
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