반응 #168585

반응 방정식

malonic acid

methylurea

acetic anhydride

→

product

수율 65.8%

1-Methylpyrimidine-2,4,6(1H,3H,5H)-trione

수율 65.8%

용매

acetic acid

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the completion of the addition
2. 2
   온도cooled to room temperature
3. 3
   기타The solvent is removed under reduced pressure
4. 4
   workup.ADDITIONthe residue is treated with 350 mL of ethanol
5. 5
   기타to precipitate out yellowish solid
6. 6
   기타The solid is recrystallized from ethanol

실험 절차

To a solution of malonic acid (80 g, 0.79 mol) and methylurea (50 g, 0.68 mol) in 180 ml of acetic acid at 70° C., acetic anhydride (130 ml, 1.37 mol) is added slowly. After the completion of the addition, the reaction mixture is stirred at 90° C. for 3 hours, and then cooled to room temperature. The solvent is removed under reduced pressure, and the residue is treated with 350 mL of ethanol to precipitate out yellowish solid. The solid is recrystallized from ethanol to give 63.1 g product as crystalline solids (Yield: 65.8%). m.p.=131.2-133.1° C. [Lit.1: m.p.=130-131.5° C.].

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