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
- 0 °C
PROCEDURE
实验过程
A slurry of 1-(2-cyanoacetyl)-1-cyclohexylmethyl-3-propylurea from above (7.10 g, 26.8 mmol) in water (45 mL)-ethanol (15 mL) was heated to 100° C. (oil bath), with adjustment of the pH to 10 by the addition of solid sodium carbonate. The resulting yellow solution was stirred for 1 h, during which time white crystalline solids formed. After 1 h 40 min, the mixture was cooled to 0° C. (icebath), and the white crystals were filtered off, washed with water (3×15 mL), and air-dried to provide 6-amino-3-(cyclohexylmethyl)-1-propyluracil as a slightly moist crystalline solid (8.85 g, quantitative yield). A small portion of this material was dried at 0.1 Torr to provide an analytically pure sample, m.p. 121°-122° C.; 1H-NMR (DMSO-d6) consistent with structure.
WORKUP
后处理
- customformed
- waitAfter 1 h 40 min
- filtrationthe white crystals were filtered off
- washwashed with water (3×15 mL)
- customair-dried