HRID2373357

反应详情

EQUATION

反应方程式

HRID 2373357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 2-(4-ethoxy-4-oxobutanamido)-5-iodobenzoate (ii-a) (22.0 g, 54 mmol) in 125 mL of THF was added a 1 M solution of KOt-Bu in THF (119 mL, 119 mmol). The reaction was complete after 2.5 h at 22° C. H2O (250 mL) and 1N HCl (60 mL) were added to the solution, and the resulting precipitate was filtered, washed with 2×50 mL Et2O, and dried in vacuo to give iii-a (16.1 g, 83%) as a whitish/gray solid as a mixture of ethyl and methyl esters: MS m/z═374 (M+H) and 360 (M+H).

WORKUP

后处理

  1. filtrationthe resulting precipitate was filtered
  2. washwashed with 2×50 mL Et2O
  3. customdried in vacuo
  4. customto give iii-a (16.1 g, 83%) as a whitish/gray solid