HRID2292661

反应详情

EQUATION

反应方程式

HRID 2292661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2-chloro-4-methylphenol (100 g), triethylamine (92.3 g) and anhydrous tetrahydrofuran (1 liter) was added dropwise pivalic chloride (93.0 g) at 5° to 10° C. under stirring over 1 hour. Then, after stirring at the same temperature for 3 hours, the reaction mixture was poured into ice water, which was extracted with diethyl ether. The organic layer was washed with 3% aqueous hydrochloric acid solution and then water, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting oil was distilled under reduced pressure, which afforded 155.3 g of 2-chloro-4-methylphenyl 2,2-dimethylpropanoate as a colorless clear liquid. Yield, 97.7%.

WORKUP

后处理

  1. stirringThen, after stirring at the same temperature for 3 hours
  2. extractionwas extracted with diethyl ether
  3. washThe organic layer was washed with 3% aqueous hydrochloric acid solution
  4. dry with materialwater, dried with anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. distillationThe resulting oil was distilled under reduced pressure, which