2,4(1H,3H)-Pyrimidinedione, 6-methyl-, 2-hydrazone (9CI) synthesis

6synthesis methods

Product Name:2,4(1H,3H)-Pyrimidinedione, 6-methyl-, 2-hydrazone (9CI)
CAS Number:37893-08-6
Molecular formula:C5H8N4O
Molecular Weight:140.14

6328-58-1 Synthesis

6328-58-1
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2,4(1H,3H)-Pyrimidinedione, 6-methyl-, 2-hydrazone (9CI)

37893-08-6
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Yield:37893-08-6 85%

Reaction Conditions:

with hydrazine hydrate in ethanol at 80; for 5.5 h;

Steps:

1.1.2 Step 2: Synthesis of 2-hydrazinyl-6-methyl-3,4-dihydropyrimidin-4-one (Intermediate 1) [00131] (EV-AN7477-001) (Intermediate 1)

[00132] To a stirred solution of 6-methyl-2-(methylsulfanyl)-3,4-dihydropyrimidin-4-one (11.9 g, 76.18 mmol) in EtOH (30 mL) was added hydrazine hydrate (15.75 mL, 0.32 mol) and stirred at 80 °C for 5.5 h. The reaction mixture was allowed to cool to r.t. and the resulting precipitate was collected and dried by vacuum filtration, washing with water (3 mL) to afford the title compound (9.20 g, 85%) as an off white powder. [00133] Method A: LC-MS m/z = 140.90 [M + H]⁺; RT = 0.18 min.

References:

WO2017/59191,2017,A1 Location in patent:Paragraph 00130-00133