HRID1458645

反应详情

EQUATION

反应方程式

HRID 1458645 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.8 g (5 mmol) of 4-(cis-4-tert-butylcyclohexylamino)-6-ethyl-5-iodopyrimidine (Example 1) and 1.0 g of copper(I) cyanide were stirred at 200° C. for 30 minutes without solvent. After cooling, the mixture was taken up in water/dichloromethane, the organic phase was again extracted by stirring with aqueous ammonia solution, and the extract was dried and concentrated. The crude product was purified by chromatography on silica gel using petroleum ether/ethyl acetate (7:3), to give 750 mg (52.4% of theory) of a colorless oil which crystallized on standing.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionthe organic phase was again extracted
  3. customthe extract was dried
  4. concentrationconcentrated
  5. customThe crude product was purified by chromatography on silica gel
  6. customto give 750 mg (52.4% of theory) of a colorless oil which
  7. customcrystallized