HRID1741553

反应详情

EQUATION

反应方程式

HRID 1741553 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-bromobutane (18.0 g, 0.13 mol) in acetone (30 ml) was added dropwise to a stirred refluxing mixture of 2-fluoro-4-hydroxybenzonitrile (15.0 g, 0.11 mol) and potassium carbonate (46.0 g, 0.33 mol) in acetone (300 ml). The stirred mixture was heated under reflux for 21 h (glc analysis revealed absence of starting material). The product was extracted into ether (twice), and the combined ethereal extracts were washed with water, 5% sodium hydroxide, water and dried (MgSO4). The solvent and the excess of 1-bromobutane were removed in vacuo to yield a pale-orange solid.

WORKUP

后处理

  1. temperaturerefluxing
  2. temperatureThe stirred mixture was heated
  3. temperatureunder reflux for 21 h (glc analysis revealed absence of starting material)
  4. extractionThe product was extracted into ether (twice), and the combined ethereal extracts
  5. washwere washed with water, 5% sodium hydroxide, water
  6. dry with materialdried (MgSO4)
  7. customThe solvent and the excess of 1-bromobutane were removed in vacuo
  8. customto yield a pale-orange solid