HRID1644802

反应详情

EQUATION

反应方程式

HRID 1644802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

TFA (4 mL) was added to the solution of (rac)-2-[(2-chloro-benzylamino)-methyl]-2-methyl-pyrrolidine-1-carboxylic acid tert-butyl ester (0.4 g) in DCM (15 mL) at 0° C. and stirred the reaction mixture at rt for 12 h. The reaction was monitored by TLC. After completion, the reaction mixture was concentrated under reduced pressure using a rotary evaporator and washed with ether (3×10 mL). The crude was basified with sodium bicarbonate and the aqueous layer was extracted with DCM (3×50 mL). The organic layer was dried over anhydrous Na2SO4 and distilled using rotary evaporator to give the desired (2-chloro-benzyl)-((rac)-2-methyl-pyrrolidin-2-ylmethyl)-amine as a sticky solid (Yield 40-70%).

WORKUP

后处理

  1. concentrationAfter completion, the reaction mixture was concentrated under reduced pressure
  2. customa rotary evaporator
  3. washwashed with ether (3×10 mL)
  4. extractionthe aqueous layer was extracted with DCM (3×50 mL)
  5. dry with materialThe organic layer was dried over anhydrous Na2SO4
  6. distillationdistilled
  7. customevaporator