HRID1158142

反应详情

EQUATION

反应方程式

HRID 1158142 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 [3-(4-fluoro-phenyl)-propyl]-methyl-carbamic acid tert-butyl ester (0.417 g, 1.560 mmol) in 3 mL of dichloromethane, was added trifluoroacetic acid (3 mL). After stirring at room temperature for 3 h, the reaction mixture was concentrated under reduced pressure. The residue was re-dissolved in 20 mL of ethyl acetate and the resulting solution was washed with NaOH solution (1N) and brine, and dried over anhydrous Na2SO4. Removal of the solvent under reduced pressure provided the title compound as a colorless oil (0.189 g, 72% yield), which was used directly in the next step (Step d of Specific Scheme 7) without further purification. GC-MS: tR=5.6 min; m/z 167 (M+).

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. dissolutionThe residue was re-dissolved in 20 mL of ethyl acetate
  3. washthe resulting solution was washed with NaOH solution (1N) and brine
  4. dry with materialdried over anhydrous Na2SO4
  5. customRemoval of the solvent under reduced pressure