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6-Chloro-1H-pyrazolo[3,4-d]pyrimidin-4(7H)-one synthesis

2synthesis methods
-

Yield: 55%

Reaction Conditions:

with sodium hydroxide in 1,4-dioxane;water at 100; for 1.5 h;

Steps:

1
[0155] 6-Chloro-lH-pyrazolo[3,4-d]pyrimidin-4(5H)-one A solution of 4,6- dichloro-lH-pyrazolo[3,4-d]pyrimidine (lg, 5.3 mmol) in NaOH (2M, aq, 5 mL) and dioxane (0.5 mL) was stirred at 100 °C for 1.5h. The mixture was acidified with HC1 (6M, aq) to pH 6.5 at 0 °C and stirred for 30 min. The reaction mixture was filtered, and the filter cake was washed with cold H2O (10 mL) and dried to obtain the product as a white solid (500 mg, (0243) 55%). (0244) [0156] MS (ES+) C5H3CIN4O requires: 170, found: 171 [M+H]+. (0245) [0157] NMR (500 MHz, DMSO-de) δ 13.92 (s, 1H), 12.89 (s, 1H), 8.68 (s, 1H).

References:

BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSYTEM;CZAKO, Barbara;JONES, Philip;CROSS, Jason;LEONARD, Paul WO2017/156397, 2017, A1 Location in patent:Paragraph 0155-0157