HRID717761

反应详情

EQUATION

反应方程式

HRID 717761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
15 °C

PROCEDURE

实验过程

To a stirred solution of 3-(4-fluorophenyl)-6-methyl-1-nitroso-1,2,3,4-tetrahydroquinoline (0.28 g, 0.00103 mol) in acetone (15 mL) was added saturated ammonium chloride solution (0.6 mL), and water (0.6 mL) at RT. The resulting brown colored reaction mixture was cooled to 15° C. Zinc dust (0.269 g, 0.00414 mol) was added portionwise at the same temperature, and after the addition, the reaction mixture was stirred for 1 h at RT. The reaction was monitored by TLC. After completion, solvent was removed under reduced pressure and the residue extracted with EtOAc (3×100 mL). The organic layer was dried over anhydrous sodium sulfate, solvent was removed under reduced pressure to obtain product as a brown colored oil (0.27 g, 92.7% yield).

WORKUP

后处理

  1. additionafter the addition
  2. customAfter completion, solvent was removed under reduced pressure
  3. extractionthe residue extracted with EtOAc (3×100 mL)
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate, solvent
  5. customwas removed under reduced pressure