HRID378507

反应详情

EQUATION

反应方程式

HRID 378507 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a stirred solution of 20.0 grams (0.12 mole) of ethyl 4-hydroxybenzoate in 200 mL of acetic acid was added a solution of 7.5 mL (excess) of 70% nitric acid in 30 mL of acetic acid. After the reaction mixture stirred for about one hour, it gradually turned orange and warmed to about 40° C. The reaction mixture was stirred for an additional eighteen hours and then was poured into 800 mL of ice-water. The mixture was stirred until the ice melted, and filtered to collect a solid, which was dissolved in ethyl acetate and dried with magnesium sulfate. The mixture was filtered, and the filtrate was concentrated under reduced pressure, yielding 22.0 grams of ethyl 3-nitro-4-hydroxybenzoate, mp 70-71° C. The NMR spectrum was consistent with the proposed structure.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred for an additional eighteen hours
  2. filtrationfiltered
  3. customto collect a solid, which
  4. dissolutionwas dissolved in ethyl acetate
  5. dry with materialdried with magnesium sulfate
  6. filtrationThe mixture was filtered
  7. concentrationthe filtrate was concentrated under reduced pressure