HRID1060263

反应详情

EQUATION

反应方程式

HRID 1060263 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

To a solution of 2-amino-4-methoxy-7-phenyl-benzothiazole (100 mg, 0.4 mmol) in pyridine (2 ml) was added benzoyl chloride (55 mg, 0.4 mmol) and the mixture stirred overnight at 20 ° C. To this mixture 2N HCl to pH 1 (20 ml) was added then the mixture was extracted twice with EtOAc (20 ml), washed with saturated NaHCO3 solution, dried with Na2SO4 and the solvent evaporated. The crude product was then chromatographed over SiO2 (Merck 230-400 mesh) eluting with CH2Cl2/MeOH (98:2), the product fractions were pooled and the solvent evaporated, to afford the title compound as a white solid (97 mg, 69% yield), MS: m/e=360 (M+).

WORKUP

后处理

  1. extractionthe mixture was extracted twice with EtOAc (20 ml)
  2. washwashed with saturated NaHCO3 solution
  3. dry with materialdried with Na2SO4
  4. customthe solvent evaporated
  5. customThe crude product was then chromatographed over SiO2 (Merck 230-400 mesh)
  6. washeluting with CH2Cl2/MeOH (98:2)
  7. customthe solvent evaporated