HRID2095428

反应详情

EQUATION

反应方程式

HRID 2095428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

In a oven-dried flask, 4-[2-(phenylacetoxy)ethyl]piperidine (101 mg, 0.41 mmol) and InBr3 (290 mg, 0.82 mmol, 2 equiv.) were dissolved in toluene (2 mL). After degassing and replacement of the atmosphere with Ar, Et3SiH (260 μL, 1.64 mmol, 4 equiv.) was added. The mixture was stirred at 90° C. for 4 h. After cooling to room temperature, the reaction was quenched with 1N HCl. After the aqueous layer was washed with EtOAc, its pH was raised to 9-10. After extraction with CH2Cl2, the organic layer was dried with Na2SO4. The solvent was removed to afford 4-[2-(2-phenylethoxy)ethyl]piperidine (40 mg, 42%) as a colorless oil.

WORKUP

后处理

  1. customAfter degassing
  2. temperatureAfter cooling to room temperature
  3. customthe reaction was quenched with 1N HCl
  4. washAfter the aqueous layer was washed with EtOAc, its pH
  5. temperaturewas raised to 9-10
  6. extractionAfter extraction with CH2Cl2
  7. dry with materialthe organic layer was dried with Na2SO4
  8. customThe solvent was removed