HRID1478803

反应详情

EQUATION

反应方程式

HRID 1478803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A suspension of N-(4-chloro-2-cyclopropylphenyl)acetamide (689 mg, 3.29 mmol) in 2M HCl (aq) (25 ml, 823 mmol) was stirred at 100° C. for 3 hrs and then 90° C. for 16 hrs. The resulting mixture was cooled to RT, diluted with EtOAc and water and the layers separated. The organic layer was extracted with 0.1 M HCl (aq) and the organic portion was discarded. To the combined aqueous portions was added 2M NaOH (aq) until basic and resulting mixture was extracted with EtOAc (2×). The organic extracts were washed with brine, dried over MgSO4, filtered and concentrated under vacuum to give the title compound as a dark yellow oil.

WORKUP

后处理

  1. wait90° C. for 16 hrs
  2. temperatureThe resulting mixture was cooled to RT
  3. customthe layers separated
  4. extractionThe organic layer was extracted with 0.1 M HCl (aq)
  5. additionTo the combined aqueous portions was added 2M NaOH (aq) until basic and
  6. customresulting mixture
  7. extractionwas extracted with EtOAc (2×)
  8. washThe organic extracts were washed with brine
  9. dry with materialdried over MgSO4
  10. filtrationfiltered
  11. concentrationconcentrated under vacuum