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2-Hydrazino-5,6-dimethylpyrimidin-4(3{H})-one synthesis

3synthesis methods
-

Yield:59224-10-1 68.2%

Reaction Conditions:

with hydrazine hydrate at 20 - 100;

Steps:

6.2 Step 2: Synthesis of 2-hydrazinyl-5,6-dimethyl-3,4-dihydropyrimidin-4-one

[00417] To 5,6-dimethyl-2-(methylsulfanyl)-3,4-dihydropyrimidin-4-one (EV-AB8059- 001, 1 g, 5.87 mmol) was added hydrazine hydrate (1.43 mL, 29.37 mmol) and stirred at 100 °C for 1.5 h. The reaction was then allowed to stand at r.t. over the weekend. A further portion of hydrazine hydrate (1.43 mL, 29.37 mmol) was added and stirred at 100 °C for 1 h. The reaction mixture was cooled to r.t. and ice cold methanol (3 mL) was added. The resultant precipitate was collected by vacuum filtration and washed with more ice cold methanol (5 mL). The solid was dried further under vacuum to afford the title compound (618 mg, 68.2%) as a white powder. [00418] Method A: LC-MS m/z = 154.9 [M + H]+; RT = 0.17 min.

References:

WO2017/59191,2017,A1 Location in patent:Paragraph 00415-00418