HRID33912

反应详情

EQUATION

反应方程式

HRID 33912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-[1-Methyl-3-(4-triisopropylsilanyloxymethyl-phenyl)-1H-pyrazol-4-yl]-pyridine (1.75 g) in THF (16.2 mL) was added TBAF (1.0M THF, 5.2 mL) and the reaction mixture stirred at ambient temperature under inert atmosphere for 1 h. The reaction mixture was poured into saturated sodium bicarbonate, extracted 3× with chloroform, dried magnesium sulfate filtered and concentration. Purification via MPLC biotage chromatography eluting with 2% methanol/0.5% saturated ammonium hydroxide/50% ethyl acetate/hexanes provided the title compound (920 mg, 84%). MS: (M+H m/z=266.1).

WORKUP

后处理

  1. extractionextracted 3× with chloroform, dried magnesium sulfate
  2. filtrationfiltered
  3. concentrationconcentration
  4. customPurification via MPLC biotage chromatography
  5. washeluting with 2% methanol/0.5% saturated ammonium hydroxide/50% ethyl acetate/hexanes