HRID68556

反应详情

EQUATION

反应方程式

HRID 68556 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

13.3 g tert-butyl 1-piperazinecarboxylate and 11.2 mL DIPEA were added to 10 g 4, 6 dichloro pyrimidine in 1000 mL dichlormethane was stirred over the weekend at RT. The solvent was removed. The residue was dissolved in 200 mL dichlormethane and 200 mL trifluoro acetic acid was added. The reaction was stirred at RT. The solvent was removed. The residue was dissolved in methanol and passed through HCO3 containing resin. The solvent was removed and the residue was purified by chromatographie on silica (dcyclohexane: ethylacetate 0-40%) to yield 13.07 g of the desired product.

WORKUP

后处理

  1. customThe solvent was removed
  2. dissolutionThe residue was dissolved in 200 mL dichlormethane
  3. addition200 mL trifluoro acetic acid was added
  4. stirringThe reaction was stirred at RT
  5. customThe solvent was removed
  6. dissolutionThe residue was dissolved in methanol
  7. customThe solvent was removed
  8. customthe residue was purified by chromatographie on silica (dcyclohexane: ethylacetate 0-40%)