HRID252107

反应详情

EQUATION

反应方程式

HRID 252107 的结构方程式

PROCEDURE

实验过程

Add trifluoroacetic acid (5 mL) to a solution of [1-(6-fluoropyridin-3-yl)-pyrrolidin-3-yl]-carbamic acid tert-butyl ester (840 mg, 3.0 mmol) in dichloromethane (5 mL). Stir for 1 h then concentrate to dryness. Dissolve the residue in methanol and pass through a column of Dowex® 1x2-200 (Cl− form). Concentrate the residue and crystallize from methanol and acetone to give (S)-1-(6-fluoropyridin-3-yl)-pyrrolidin-3-ylamine hydrochloride as a tan solid (453 mg, 70%).

WORKUP

后处理

  1. concentrationthen concentrate to dryness
  2. dissolutionDissolve the residue in methanol
  3. concentrationConcentrate the residue
  4. customcrystallize from methanol and acetone