HRID588093

反应详情

EQUATION

反应方程式

HRID 588093 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6-chloro-3-iodo-1H-pyrazolo[4,3-c]pyridine (1.874 g, 6.71 mmol) in THF (20 mL) was treated with NaH (60% in mineral oil; 0.402 g, 10.06 mmol) at 0° C. and the mixture was stirred for 50 min. Trityl chloride (2.244 g, 8.05 mmol) was added at 0° C. and the mixture was stirred for 16 h at room temperature, quenched with saturated NH4Cl, and extracted with EtOAc. The organic phase was washed with water, brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified via flash chromatography (0-10% EtOAc-hexanes) to yield 6-chloro-3-iodo-1-trityl-1H-pyrazolo[4,3-c]pyridine. MS ESI calc'd. for C25H18ClIN3[M+1]+ 522. found 522.

WORKUP

后处理

  1. stirringthe mixture was stirred for 16 h at room temperature
  2. customquenched with saturated NH4Cl
  3. extractionextracted with EtOAc
  4. washThe organic phase was washed with water, brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified via flash chromatography (0-10% EtOAc-hexanes)