NSC45719 synthesis

Yield:6632-63-9 92.9%

Reaction Conditions:

with sodium hydroxide in water at 120; for 5 h;

Steps:

3

Step 3 : A mixture of 4,6-dichloro-2-(methylthio)pyrimidine (5.0 g, 25.6 mmol) in aqueous NaOH (2N, 120 mL) was stirred at 120 °C for 5 hours. The reaction mixture was cooled to 20 °C and AcOH was added until pH = 6. The resulting precipitate was filtered off and washed with water. The solid was triturated with petroleum ether (30 mL), filtered, and dried in vacuo to afford 6-chloro-2-(methylthio)pyrimidin-4-ol (4.2 g, 92.9% yield) as a white solid: ¹HNMR (400 MHz, methanol-r) d 6.23 (s, 1H), 2.59 (s, 3H).

References:

WO2019/165073,2019,A1 Location in patent:Paragraph 0368; 0370