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5,6-DIHYDROXY-2-PYRIDIN-2-YL-PYRIMIDINE-4-CARBOXYLIC ACID METHYL ESTER synthesis

5synthesis methods
-

Yield:-

Reaction Conditions:

Stage #1: dimethyl acetylenedicarboxylate;N'-hydroxypyridine-2-carboximidamide in chloroform at 65; for 1 h;
Stage #2: in 5,5-dimethyl-1,3-cyclohexadiene at 140; for 3 h;Dean-Stark;

Steps:



[00541] Step B: To a suspension of compound 50 (5.0 g, 1 eq) in CHCI3 (100 mL), compound 51 (5.2 g, 1 eq) was added. The resulting mixture was heated at 65°C for 1 h and filtered. The solvent was evaporated in vacuo and the residue was taken up with xylene (50 mL). The resulting mixture was heated at 140°C with a Dean - Stark trap for 3 h. The reaction mixture was cooled to 25°C, the precipitate was filtered and washed with MTBE (2*20 mL) and dried to obtain compound 52 (4.1 g, 90+% purity).

References:

WO2020/132071,2020,A1 Location in patent:Paragraph 00541

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