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ChemicalBook CAS DataBase List Ethyl 3,3-Diethoxypropionate
10601-80-6

Ethyl 3,3-Diethoxypropionate synthesis

15synthesis methods
Ethyl 3,3-diethoxypropionate can be used as organic synthesis intermediates and pharmaceutical intermediates for the synthesis of coumarin and other compounds. Ethyl 3,3-diethoxypropionate is synthesised by that 1,1,1-trichloro-4-ethoxy-3-buten-2-one in ethanol with anhydrous potassium carbonate was stirred for 10 h at RT to give it.
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Yield:10601-80-6 84.5%

Reaction Conditions:

with potassium carbonate at 10 - 60; for 10 h;

Steps:

1 The method of preparing a 3,3-alkoxy-propionate
Into a flask, 868 g of anhydrous ethanol and 27.6 g (0.2 mol) of anhydrous potassium carbonate were charged, and while stirring and ice-cooling to 10 ° C, 217 g (1 mol) of 1,1,1-trichloro-4-ethoxy- Butene-2-one in a flask, and then the temperature was raised to 60 ° C and the reaction was stirred10h. Excess ethanol was distilled off under reduced pressure, filtered and the filtrate was distilled under reduced pressure to give 160.5 g of ethyl 3,3-diethoxypropionate (93-96C, 15 mmHg) as a light yellow or colorless transparent liquid in a yield of 84.5 %. IR, NMR and MS data of the target product are as follows: IR (cm-1): 2990,2940,1740,1115,1060.1HNMR (400MHz, CDCl3) δ (ppm): 1.18 (t, 6H, J = 7, 2H, J = 6,2-H), 3.30-3.80 (4H, 2OCH2CH3), 4.13 (q, 2H, J = 7, CO2CH2CH3) , 4.93 (t, 1H, J = 6,3-H). FAB-MS (m / z): 191 [M + H] +.

References:

Tailite Pharmaceutical (Hubei) Co., Ltd.;Liu Mingxing;Wu Jianhong CN107056608, 2017, A Location in patent:Paragraph 0025

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