HRID2035683

反应详情

EQUATION

反应方程式

HRID 2035683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-(Pyridine-3-yloxy)benzaldehyde (0.500 g, 2.510 mmol), 4-acetamidobenzene sulfonyl azide (0.724 g, 3.01 mmol), dimethyl (2-oxopropyl) phosphonate (0.412 mL, 3.01 mmol), and potassium carbonate (1.041 g, 7.53 mmol) in MeCN (10.5 mL) and MeOH (2.1 mL) was heated to 40° C. for 16 h while under N2. The solvent was removed and residue was redissolved in EtOAc and washed with water (3×) and brine (1×). The organic phase was separated, dried with Na2SO4 and evaporated to afford an oil. This material was chromatographed on silica (0-80% EtOAc in hexanes) to yield 0.238 g as an oil.

WORKUP

后处理

  1. customThe solvent was removed
  2. dissolutionresidue was redissolved in EtOAc
  3. washwashed with water (3×) and brine (1×)
  4. customThe organic phase was separated
  5. dry with materialdried with Na2SO4
  6. customevaporated
  7. customto afford an oil
  8. customThis material was chromatographed on silica (0-80% EtOAc in hexanes)
  9. customto yield 0.238 g as an oil