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113885-20-4

2,4(1H,3H)-PYRIMIDINEDIONE, 6-AMINO-1-(1-METHYLETHYL)- synthesis

3synthesis methods
-

Yield:-

Reaction Conditions:

with sodium in isopropyl alcohol at 95;Inert atmosphere;

Steps:

1.1 Intermediate 1 .1

The reaction was performed under argon atmosphere and in dried glassware. Na (4.50 g, 196 mmol) was added in pieces to dry propan-2-ol (150 mL). The mixture was stirred for 2 h and heated to 95 °C. After the Na was completely dissolved, isopropyl-urea (10.0 g, 97.9 mmol) and cyano-acetic acid ethyl ester (10.4 mL, 97.9 mmol) were added and the mixture was stirred overnight at 95 °C. The mixture was cooled down and H2O (40.0 mL) was added and the pH was adjusted to 6 with cone HCI. Stirring was continued under ice cooling and N2atmosphere for 12 h. The obtained precipitate was filtered and dried to obtain the product.MS (ESI+): (M+H)+170HPLC: RT = 0.23 min, Method F

References:

WO2019/11802,2019,A1 Location in patent:Page/Page column 25