HRID2285613

反应详情

EQUATION

反应方程式

HRID 2285613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of sodium hydride (4.32 g., 0.09 mole, 50% suspension in mineral oil) in 50 ml. of dimethylformamide was added by dropwise addition acetaldoxime (5.31 g., 0.09 mole) at 5°. The mixture was stirred for 10 minutes at 20°-25° and then treated by dropwise addition with a solution of 10 g. (0.03 mole) of ethyl 4-(4-nitrobenzoyl) phenoxy acetate in 50 ml. of dimethylformamide. The resulting mixture was stirred at room temperature for 5 hrs. and poured into cold water. Acidification with concentrated hydrochloric gave a solid which was collected by filtration and dried. There was obtained 7 g. of product. This material was used without purification for the next step. In a similar manner were prepared the following two compounds: 4-(4-hydroxybenzoyl)-2-chlorophenoxy acetic acid and 4-(4-hydroxybenzoyl)-3-chlorophenoxy acetic acid.

WORKUP

后处理

  1. additiontreated by dropwise addition with a solution of 10 g
  2. stirringThe resulting mixture was stirred at room temperature for 5 hrs
  3. concentrationAcidification with concentrated hydrochloric
  4. customgave a solid which
  5. filtrationwas collected by filtration
  6. customdried
  7. customThere was obtained 7 g
  8. customThis material was used without purification for the next step
  9. customIn a similar manner were prepared the following two compounds