HRID1250096

反应详情

EQUATION

反应方程式

HRID 1250096 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tert-butyl bromoacetate (75 g, 385 mmol) was added to a solution/suspension of 3-hydroxymethyl-2-methylphenol (46.6 g, 337 mmol) and finely powdered potassium carbonate (60 g) in acetone (500 mL). The mixture was heated at reflux for about 40 hours or until the reaction was complete. The solids were filtered, and the liquid residue was evaporated. Purification of the residue by silica gel chromatography, eluting with acetone/hexane, gave (3-hydroxymethyl-2-methylphenoxy)acetic acid tert-butyl ester as a pale yellow oil (80.1 g, 96%).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for about 40 hours or until the reaction
  3. filtrationThe solids were filtered
  4. customthe liquid residue was evaporated
  5. customPurification of the residue by silica gel chromatography
  6. washeluting with acetone/hexane