HRID1670836

反应详情

EQUATION

反应方程式

HRID 1670836 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Treat a solution of 4-bromo-2-cyclohexyl-N-(2,6-dichloro-4-methoxy-benzyl)-butyramide (2.0 g, 4.6 mmol) in THF (30 mL) with diisopropyl ethyl amine (1.19 g, 9.19 mmol) at 40° C. for 12 hours and at reflux for 6 hours. Cool the reaction, dilute with ethylacetate and wash with HCl (1N) and water. After drying the organic layer over sodium sulfate, filtrate and concentrate under vacuum. Purify the residue by silica gel chromatography with 1:4 ethyl acetate:hexane to afford 1.3 g (80%) of the title compound. MS (m/z): 356 (M+).

WORKUP

后处理

  1. temperatureat reflux for 6 hours
  2. temperatureCool
  3. customthe reaction
  4. washwash with HCl (1N) and water
  5. dry with materialAfter drying the organic layer over sodium sulfate, filtrate
  6. concentrationconcentrate under vacuum
  7. customPurify the residue by silica gel chromatography with 1:4 ethyl acetate