HRID844420

反应详情

EQUATION

反应方程式

HRID 844420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.77 g of 4-cyclohexanebutyryl chloride dissolved in 10 ml of CCl4 are added to a suspension of 2.8 g of AlCl3 in 20 ml of CCl4 at +4° C. under nitrogen. 5.2 g of 2,5-dimethoxychlorobenzene in 10 ml of CCl4 are added dropwise and the mixture is then left stirring for 3 hours at RT. The reaction medium is hydrolysed with dilute HCl solution, the phases are then separated by settling and the organic phase is extracted with DCM. After drying over MgSO4, the solution is evaporated and the residue is then purified by chromatography on silica, eluting with a heptane/DCM mixture (60/40; v/v) and then with pure DCM. 3.37 g of the expected compound are obtained: m.p.=80-81° C.

WORKUP

后处理

  1. waitthe mixture is then left
  2. customthe phases are then separated
  3. extractionthe organic phase is extracted with DCM
  4. dry with materialAfter drying over MgSO4
  5. customthe solution is evaporated
  6. customthe residue is then purified by chromatography on silica
  7. washeluting with a heptane/DCM mixture (60/40; v/v)