ChemicalBook CAS DataBase List Thieno[3,4-b]-1,4-dioxin-5,7-dicarboxylic acid, 2,3-dihydro-, diethyl ester

Thieno[3,4-b]-1,4-dioxin-5,7-dicarboxylic acid, 2,3-dihydro-, diethyl ester synthesis

6synthesis methods

Product Name:Thieno[3,4-b]-1,4-dioxin-5,7-dicarboxylic acid, 2,3-dihydro-, diethyl ester
CAS Number:154934-13-1
Molecular formula:C12H14O6S
Molecular Weight:286.3

3 4-DIHYDROXY-THIOPHENE-2 5-DICARBOXYLI&

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107-06-2 Synthesis

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Thieno[3,4-b]-1,4-dioxin-5,7-dicarboxylic acid, 2,3-dihydro-, diethyl ester

154934-13-1
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Yield:154934-13-1 95.9%

Reaction Conditions:

in acetonitrile at 115; under 750.075 Torr; for 2.03333 h;Solvent;Temperature;

Steps:

1.1-3.4 Example 2: A method for preparing an EDOT intermediate includes the following steps:

1) 130 mL (0.5 mol) of diethyl 2,5-dicarboxylate-3,4-.dihydroxy sodium thiophene,100g (1.01mol) of 1,2-dichloroethane and 200mL of acetonitrile were placed in an airtight container.Evacuate to a vacuum of 0.1 MPa, hold for 2 minutes, heat until the temperature in the container reaches 115 ° C, and hold the reaction for 2 hours; 2) Reduce to room temperature, discharge, and recover the solvent by distillation under reduced pressure to obtain a brown oily solid; 3) Add a mixture of 50 mL of isopropanol and 300 mL of water, stir uniformly at 60 ° C, cool and filter to obtain a yellow-yellow solid; 4) Add 400 mL of water and stir for an additional 1 h to obtain 275 g of a wet earthy yellow solid, which is dried to obtain diethyl 2,5-dicarboxylate-3,4-ethylenedioxythiophene.After drying, 137.3 g of the target product was obtained with a yield of 95.9% and a purity of more than 97%.

References:

CN110615799,2019,A Location in patent:Paragraph 0043; 0049-0066