Reaktion #88617

Reaktionsgleichung

1-methylurea

4-methyleneoxetan-2-one

→

1,6-dimethylpyrimidine-2,4(1H,3H)-dione

Ausbeute 18.0%

Lösungsmittel

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe reaction was filtered
2. 2
   Waschenthe filtered solid was washed with MeOH (20 mL)
3. 3
   Sonstigedried

Vorschrift

A solution of 1-methylurea (30 g, 0.356 mol) in 4-methyleneoxetan-2-one (26.4 g, 0.356 mol) was heated at 100° C. for 18 h, cooled to RT then diluted with MeOH (50 mL). The reaction was filtered and the filtered solid was washed with MeOH (20 mL) and dried to give 1,6-dimethylpyrimidine-2,4(1H,3H)-dione (9 g, 18% yield) as a white solid. 1H NMR (CDCl3) δ: 8.33 (s, 1H), 5.58 (s, 1H), 3.38 (s, 3H), 2.26 (s, 3H). LCMS: MH+ 141 and TR=0.368 min. Used without further purification.

Quelle