HRID869534

反应详情

EQUATION

反应方程式

HRID 869534 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[step 1] Commercially available 3-chloro-2-nitroaniline (3.0 g, 17 mmol) was dissolved in DMF (87 mL), sodium thiomethoxide (1.54 g, 21 mmol) was added, and the mixture was stirred at room temperature for 3 hr. The reaction was discontinued with water, and the mixture was extracted with ethyl acetate, and the extract was dried over sodium sulfate and filtered. The filtrate was concentrated under reduced pressure. The residue was crystallized from isopropyl ether to give 3-(methylthio)-2-nitroaniline (2.5 g, 78%).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialthe extract was dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customThe residue was crystallized from isopropyl ether