HRID598111

反应详情

EQUATION

反应方程式

HRID 598111 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

Diisopropyl amine (0.16 mL, 1.13 mmol) was dissolved in tetrahydrofuran (2 mL). n-Butyllithium (2.5M, 0.45 mL, 1.13 mmol) was added at 0° C. and the reaction stirred for 0.5 h. The solution was cooled to −78° C. and 1-(6-mesityl-pyridin-2-yl)-pentan-2-one (0.29 g, 1.0 mmol) was added. After 0.5 h, ethyl ethoxymethylene malonate (0.21 mL, 1.0 mmol) was added and the reaction was warmed to room temperature. The solution was quenched with water, extracted with ethyl acetate, dried, and concentrated. Flash chromatography (10%-20% ethyl acetate/hexanes) gave the title compound as a mixture of two isomers.

WORKUP

后处理

  1. waitAfter 0.5 h
  2. temperaturethe reaction was warmed to room temperature
  3. customThe solution was quenched with water
  4. extractionextracted with ethyl acetate
  5. customdried
  6. concentrationconcentrated