HRID905325

反应详情

EQUATION

反应方程式

HRID 905325 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 6-methylaminopurine (7.45 g, 50 mmols), potassium carbonate (6.9 g, 50 mmols) and N,N-dimethylacetamide (250 ml) was added 2-chloro-6-fluorobenzyl chloride (17.9 g, 100 mmols), and the resultant mixture was allowed to react at 110° C. for 6 hours with stirring. After cooling, the reaction mixture was filtered to remove insoluble materials and the filtrate was concentrated to dryness under reduced pressure. Upon addition of water to the resultant residue, the formed precipitate was collected by filtration and recrystallized from ethanol to give 9-(2-chloro-6-fluorobenzyl)-6-methylaminopurine as colorless needles (9.08 g, yield 63%), m.p. 188°-190° C.

WORKUP

后处理

  1. customto react at 110° C. for 6 hours
  2. temperatureAfter cooling
  3. filtrationthe reaction mixture was filtered
  4. customto remove insoluble materials
  5. concentrationthe filtrate was concentrated to dryness under reduced pressure
  6. additionUpon addition of water to the resultant residue
  7. filtrationthe formed precipitate was collected by filtration
  8. customrecrystallized from ethanol