HRID599672

反应详情

EQUATION

反应方程式

HRID 599672 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 6-iodo-benzo[b]thiophene-2-carboxylic acid ethyl ester (2.95 g, 8.88 mmol) in THF (60 mL) at −78° C. is added ethylmagnesium bromide (4.45 mL, 3.0 M). The reaction mixture is stirred for 15 min, and 3-pentanone (3.0 mL) is added. The mixture is allowed to warm to RT and stirred for 30 min. The reaction is quenched with HCl (15 mL, 1.0 M) and extracted with EtOAc (2×50 mL). The organic layer is dried over Na2SO4, concentrated, and purified by silica gel column chromatography to give the title compound (0.65 g, 25%).

WORKUP

后处理

  1. stirringstirred for 30 min
  2. customThe reaction is quenched with HCl (15 mL, 1.0 M)
  3. extractionextracted with EtOAc (2×50 mL)
  4. dry with materialThe organic layer is dried over Na2SO4
  5. concentrationconcentrated
  6. custompurified by silica gel column chromatography