HRID716043

反应详情

EQUATION

反应方程式

HRID 716043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a 100 ml three necked round bottom flask 1-(2-(5-(hydroxymethyl)pyridin-2-ylamino)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazin-7-yl)-2,2-dimethylpropan-1-one (0.5 g, 0.00109 mole) was taken in CH2Cl2 (20 ml). MnO2 (1.9 g, 0.0219 mole) was added in one portion at room temperature under nitrogen atmosphere. The reaction mixture was stirred for 15 min. After completion of the reaction, the reaction mixture was filtered through celite bed and washed with CH2Cl2. The filtrate was collected and concentrated to afford crude product which was subjected for the column purification. The crude compound was purified using column purification by eluting the compound with 25-30% ethyl acetate in hexanes to yield 0.33 g of 6-(7-pivaloyl-5-((2-(trimethylsilyl)ethoxy)-methyl)-5H-pyrrolo[2,3-b]pyrazin-2-ylamino)nicotinaldehyde.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. filtrationthe reaction mixture was filtered through celite bed
  3. washwashed with CH2Cl2
  4. customThe filtrate was collected
  5. concentrationconcentrated
  6. customto afford crude product which
  7. customwas subjected for the column purification
  8. customThe crude compound was purified
  9. customcolumn purification
  10. washby eluting the compound with 25-30% ethyl acetate in hexanes