HRID1879119

反应详情

EQUATION

反应方程式

HRID 1879119 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

n-Butyllithium (11.7 ml, 18.77 mmol) was added dropwise to a solution of 4-chloro-2-fluoroanisole (2.01 g, 12.52 mmol) in tetrahydrofuran (20 ml) at −78° C. and the reaction was stirred for 30 mins. Crushed solid carbon dioxide was added in one portion and the reaction was then allowed to warm to room temperature. The solvent was evaporated and the residue dissolved in water. Sodium hydroxide (2M to pH˜14) was added and the aqueous layer extracted with ethyl acetate. The aqueous layer was acidified with hydrochloric acid (5M, pH˜1) and the title compound was collected as a colourless solid (2.25 g, 88%). The compound was dried in vacuo.

WORKUP

后处理

  1. additionwas added in one portion
  2. customThe solvent was evaporated
  3. dissolutionthe residue dissolved in water
  4. additionSodium hydroxide (2M to pH˜14) was added
  5. extractionthe aqueous layer extracted with ethyl acetate
  6. customthe title compound was collected as a colourless solid (2.25 g, 88%)
  7. customThe compound was dried in vacuo