3-AMino-4-broMo-thiophene-2-carboxylicacidMethylester synthesis

Yield:161833-42-7 82%

Reaction Conditions:

with bromine;acetic acid at 60; for 0.75 h;

Steps:

309.A Step A
General procedure: To a solution of compound 73 (1.0 eq) in HOAc (15.0 mL) was added Br2 (3.0 eq). The reaction was heated to 60° C. and allowed to stir approximately 45 minutes. The excess Br2 was neutralized with excess of Na2 S203, and the crude product was extracted (3 *25 mL) of DCM. The combined organic layers were dried over Mg504 and concentrated in vacuo, affording crude compound 74 as a light yellow solid. The products were used in the next step without purification. The scale of the reaction was calculated based on a theoretical yield of 1 g of 74.

References:

SHY THERAPEUTICS LLC;HADARI, Yaron R.;CARTA, Luca;SCHMERTZLER, Michael;WILLIAMS, Theresa M.;REYNOLDS, Charles H.;HUTCHESON, Rebecca WO2018/237084, 2018, A1 Location in patent:Paragraph 002139; 002644

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