HRID904139

反应详情

EQUATION

反应方程式

HRID 904139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

3-n-Butyl-5-(1-methylethylidene)-2,4-imidazolidinedione (3.8 g 0.02 mole) was added to a suspension of sodium hydride (0.95 g 50% oil dispersion 0.2 mole) in dry dimethylformamide (30 ml) and heated at 50° C. for five minutes. The mixture was cooled to room-temperature, methyl iodide (3.4 g 0.024 mole) added and the mixture heated at 50° C. for fifteen minutes. The mixture was then evaporated to dryness on a rotary evaporator under reduced pressure and the residue dissolved in water (100 ml) and extracted into ether (3×50 ml). The ethereal solution was dried (MgSO4) the solvent removed and the residue (title compound) distilled under reduced pressure in a Kugelrohr apparatus, b.p. 100° C. at 0.01 mm. Yield=3.8 g=92%.

WORKUP

后处理

  1. additionadded
  2. temperaturethe mixture heated at 50° C. for fifteen minutes
  3. customThe mixture was then evaporated to dryness on a rotary evaporator under reduced pressure
  4. dissolutionthe residue dissolved in water (100 ml)
  5. extractionextracted into ether (3×50 ml)
  6. dry with materialThe ethereal solution was dried (MgSO4) the solvent
  7. customremoved
  8. distillationthe residue (title compound) distilled under reduced pressure in a Kugelrohr apparatus, b.p. 100° C. at 0.01 mm