HRID2172715

反应详情

EQUATION

反应方程式

HRID 2172715 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lithium bis(trimethylsilyl)amide (1 M in tetrahydrofuran, 25.3 mL, 25.3 mmol) was added to a mixture of ethyl isobutyrate (2.67 g, 23.0 mmol) in tetrahydrofuran (25 mL) at −78° C. After stirring for 30 m, a solution of 2-(chloromethyl)naphthalene (400 mg, 2.30 mmol) in tetrahydrofuran (10 mL) was added to the reaction mixture dropwise. The mixture was stirred at −78° C. for another hour and then at room temperature overnight. The mixture was quenched by the addition of water and extracted with ethyl acetate. The combined organic fractions were washed with water, dried over sodium sulfate and concentrated under vacuum to give ethyl 2,2-dimethyl-3-(naphthalene-2-yl)propanoate (1.00 g) as a yellow oil, which was used without further purification.

WORKUP

后处理

  1. stirringThe mixture was stirred at −78° C. for another hour
  2. customat room temperature
  3. customovernight
  4. customThe mixture was quenched by the addition of water
  5. extractionextracted with ethyl acetate
  6. washThe combined organic fractions were washed with water
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated under vacuum