HRID2068527

反应详情

EQUATION

反应方程式

HRID 2068527 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To ethyl 1-[(4-chlorobenzoyl)amino]cyclopropanecarboxylate (157 g, 0.58 mol) in 1,4-dioxane (2.4 L), add a solution of lithium hydroxide (123.05 g, 2.93 mol) in water (1.2 L). Stir the reaction mixture at ambient temperature for 4 hours and then concentrate it under reduced pressure. Dilute the mixture with water (1 L) and immerse it in an ice water bath. Adjust the pH to approximately 2 with aqueous 5N HCl. Filter the precipitate, wash the cake with water (3×1 L), and dry (50° C., vacuum oven) to give (132 g, 94%) the title compound as a white powder: MS (m/z): 240 (M+1).

WORKUP

后处理

  1. concentrationconcentrate it under reduced pressure
  2. additionDilute the mixture with water (1 L)
  3. filtrationFilter the precipitate
  4. washwash the cake with water (3×1 L)
  5. customdry (50° C., vacuum oven)