HRID1897571

反应详情

EQUATION

反应方程式

HRID 1897571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-bromo-2-naphthoic acid (2 g, 7.97 mmol) was stirred in thionyl chloride (13.28 ml) at 70° C. for 16 h. Solvent was evaporated, and the residue was dissolved in CH2Cl2 and concentrated again. To the acid chloride intermediate was added ammonia (7N in MeOH, 13.66 ml, 96 mmol) and the mixture was stirred at room temperature for 3 h. The reaction mixture was concentrated, diluted in ethyl acetate and filtered. The solid was rinsed with ethyl acetate and then dried. The title compound 2a (1.802 g, 90%) was isolated as beige solid. LC-MS (M+1) 251.9, t=1.34 min.

WORKUP

后处理

  1. customSolvent was evaporated
  2. dissolutionthe residue was dissolved in CH2Cl2
  3. concentrationconcentrated again
  4. concentrationThe reaction mixture was concentrated
  5. additiondiluted in ethyl acetate
  6. filtrationfiltered
  7. washThe solid was rinsed with ethyl acetate
  8. customdried