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ChemicalBook CAS DataBase List 4H-Pyrazolo[3,4-d]pyrimidin-4-one, 1,5-dihydro-6-methyl- (9CI)

4H-Pyrazolo[3,4-d]pyrimidin-4-one, 1,5-dihydro-6-methyl- (9CI) synthesis

6synthesis methods
-

Yield:30129-57-8 96%

Reaction Conditions:

with sulfuric acid at 10 - 120; for 16.5 h;

Steps:

A Step A

6-methyl-1H-pyrazolo[3,4-djpyrimidin-4(5H)-one. To a stirred suspension of3-amino-lH-pyrazole-4-carbonitrile (150 g, 1.39 mol) in acetic acid (300 mL) was added H2S04(300 mL) drop wise over a period of30 min at l0°C. Reaction mixture VaS heated to 120°C for16 h. The reaction mixture was cooled to 25°C and poured into ice (l kg) and basifi.ed with a15 sat. aq. solution of Na2C03. The precipitated solid was filtered and washed w·ith water (300mL), dried under reduced pressure and co-distilled with toluene to provide the title compound(200 g, 96%) as an off-white solid. 1H N~1R (300 lVIHz, DMSO-d6) 8 13.2-12.2 (br. s., lH),8.01 (s, lH), 3.7-3.1 (br. s, 1H), 2.32 (s, 3H). [M+H] '" 151.1

References:

WO2018/125810,2018,A1 Location in patent:Page/Page column 63