HRID547589

反应详情

EQUATION

反应方程式

HRID 547589 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 2-pyridylcarbinol (10) (300 mg, 2.70 mmol) and triethyl amine (698 mg, 6.75 mmol) in dry THF (10 mL) at 0° C. was added a solution of mesylchloride (470 mg, 4.1 mmol) in dry THF (10 mL). Reaction mixture was allowed to stir for 2 h at room temperature [reaction was followed by TLC]. Reaction mixture was concentrated to remove THF under reduced pressure and the residue was dissolved in CH2Cl2 (100 mL), washed with brine, dried over anhydrous Na2SO4 and concentrated under reduced pressure to give compound 11 (300 mg, 59%) as gum and it was taken as such for next step.

WORKUP

后处理

  1. customReaction mixture
  2. custom[reaction was followed by TLC]
  3. customReaction mixture
  4. concentrationwas concentrated
  5. customto remove THF under reduced pressure
  6. dissolutionthe residue was dissolved in CH2Cl2 (100 mL)
  7. washwashed with brine
  8. dry with materialdried over anhydrous Na2SO4
  9. concentrationconcentrated under reduced pressure