HRID558115

反应详情

EQUATION

反应方程式

HRID 558115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Mix 2-(2-bromo-4-fluoro-phenyl)-2-methyl-propionitrile (1 g, 4.13 mmol) and 1,4,7,10,13,16-hexaoxacyclooctadecane (18-crown-6) (100 mg, 1% wt) with sodium hydroxide (10 M, 20 mL, 200 mmol) in ethanol (5 mL). Heat the mixture to reflux for 3 h. Quench the reaction with 1 N HCl. Extract the product with chloroform. Dry the organic phase over sodium sulfate and concentrate to give an oily residue. Purify the residue by FCC (10% methanol in DCM as eluant) to give the title compound as a yellow solid (1 g, 93%). MS (ES) m/z 260/262 [M+1]+.

WORKUP

后处理

  1. temperatureHeat the mixture
  2. temperatureto reflux for 3 h
  3. customQuench
  4. customthe reaction with 1 N HCl
  5. extractionExtract the product with chloroform
  6. dry with materialDry the organic phase over sodium sulfate
  7. concentrationconcentrate
  8. customto give an oily residue
  9. customPurify the residue by FCC (10% methanol in DCM as eluant)