HRID598184

反应详情

EQUATION

反应方程式

HRID 598184 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a suspension of N-(5,6-diiodo-7-methyl-4-oxo-4,7-dihydro-3H-pyrrolo[2,3-d]pyrimidin-2-yl)-2,2-dimethylpropanamide (941 mg, 1.88 mmol) in acetic acid (9 ml) and water (2 ml) was added zinc powder (246 mg, 3.76 mmol), and the mixture was stirred at room temperature for 1 day. After addition of zinc (123 mg, 1.88 mmol), the mixture was stirred at room temperature for 1 day. The reaction mixture was diluted with water and stirred at 0° C. for 2 hours. The resulting crystals were collected by filtration, washed with water and dissolved in tetrahydrofuran. The solution was filtrated, and the filtrate was concentrated in vacuo. The residue was washed with diiopropyl ether to give 545 mg (78%) of the title compound.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 1 day
  2. stirringstirred at 0° C. for 2 hours
  3. filtrationThe resulting crystals were collected by filtration
  4. washwashed with water
  5. dissolutiondissolved in tetrahydrofuran
  6. filtrationThe solution was filtrated
  7. concentrationthe filtrate was concentrated in vacuo
  8. washThe residue was washed with diiopropyl ether