HRID908154

反应详情

EQUATION

反应方程式

HRID 908154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Isoamyl nitrite (3.5 ml, 25 mmol) is added to a stirred suspension/solution of anhydrous copper (II) chloride (2.75 g, 20 mmol) in dry methylcyanide (50 ml). 4-Methyl-5-(4-nitro-phenyl)-thiazol-2-ylamine (25a) (4.0 g, 17 mmol) is then added over 30 minutes. The resulting slurry is stirred at room temperature for 1 hour then heated at 70° C. for 30 minutes. After cooling to room temperature the black solution is poured into 4M hydrochloric acid (200 ml). The product is extracted with ethyl acetate, dried (MgSO4) and the solvent removed to give the title compound as an orange powder (3.13 g). MH+ (TOF, ES+): 255.0

WORKUP

后处理

  1. temperaturethen heated at 70° C. for 30 minutes
  2. temperatureAfter cooling to room temperature the black solution
  3. extractionThe product is extracted with ethyl acetate
  4. dry with materialdried (MgSO4)
  5. customthe solvent removed