反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
N-Methyl-N'-phenylurea was preliminarily prepared from phenyl isocyanate and methylamine by the procedure described in Step 1. Using the urea compound as the starting material, uracil ring was formed by the procedure described in Step 2. N-Methyl-N'-phenylurea (30 g, 0.2M) and cyanoacetic acid (18.8 g, 0.22M) were dissolved in 400 ml of a solvent, acetic anhydride, and heated at 80° C. for 2 hours. The solvent acetic anhydride was distilled off under reduced pressure and 200 ml of water was added to the residue, followed by cooling with ice. A 2N aqueous solution of NaOH (220 ml) was then added and the mixture was stirred for 2 hours. A precipitated solid product was obtained by filtration. The solid product was washed successively with water and methanol and dried to yield 6-amino-3-methyl-1-phenyluracil (yield: 33 g, or 76% based on N-methyl-N'-phenylurea).
WORKUP
后处理
- customuracil ring was formed by the procedure
- distillationThe solvent acetic anhydride was distilled off under reduced pressure and 200 ml of water
- additionwas added to the residue
- temperatureby cooling with ice
- additionA 2N aqueous solution of NaOH (220 ml) was then added
- customA precipitated solid product was obtained by filtration
- washThe solid product was washed successively with water and methanol
- customdried