HRID1396885

反应详情

EQUATION

反应方程式

HRID 1396885 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 bis(1,1-dimethylethyl) 2-methyl-1,5-pyrazolidinedicarboxylate dissolved in dichloromethane (DCM) (25 mL) was added TFA (30.7 mL, 398 mmol) and water (3.59 mL, 199 mmol). The reaction was stirred at rt and monitored by LCMS. When the reaction was deemed complete, the solvent was evaporated under reduced pressure to give a residue which was azeotroped from toluene (50 mL×3) in order to remove the TFA and water. The crude product was obtained as a colorless oil (97% yield based on TFA Salt), which was used directly for the next step. LC-MS (ES) m/e 130.9 (M+H)+.

WORKUP

后处理

  1. customthe solvent was evaporated under reduced pressure
  2. customto give a residue which
  3. customwas azeotroped from toluene (50 mL×3) in order
  4. customto remove the TFA and water