HRID49327

反应详情

EQUATION

反应方程式

HRID 49327 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

15 g (81.4 mmol) of 2-ethyl-2-2-thienyl-[1,3]dioxolane are dissolved in 300 mL of anhydrous THF and the mixture is then cooled to −78° C. 53 mL (89 mmol) of 1.7 M tert-butyllithium solution are then added, after which the reaction medium is stirred for 1 hour. 10 mL (120 mmol) of anhydrous DMF are then added and the medium is stirred for 1 hour. The reaction medium is treated at −78° C. with 1N hydrochloric acid solution and is then extracted with ethyl acetate and the organic phases are combined, dried and concentrated under reduced pressure. The residue obtained is purified by chromatography on a column of silica. A yellow oil is obtained (m=19 g; Y=100%).

WORKUP

后处理

  1. stirringthe medium is stirred for 1 hour
  2. extractionis then extracted with ethyl acetate
  3. customdried
  4. concentrationconcentrated under reduced pressure
  5. customThe residue obtained
  6. customis purified by chromatography on a column of silica
  7. customA yellow oil is obtained (m=19 g; Y=100%)