HRID735843

反应详情

EQUATION

反应方程式

HRID 735843 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 3-bromo benzoic acid (10 g, 0.5 mol), silver carbonate (276 g, 1 mol) and dry molecular sieves (100 g) taken in dry CH2Cl2 (2 L), tert-butylbromide (115 mL, 1 mol) was added dropwise at 0° C. and the reaction mixture was stirred overnight at RT. The solid was filtered and washed with dichloromethane. Organic layer was washed with 10% aqueous solution of NaHCO3 (2×500 mL), water (2×500 mL), brine and dried. The solvent was removed under vacuum to give tert-butyl-3-bromobenzoate (70 g, 57%).

WORKUP

后处理

  1. customdry molecular sieves (100 g)
  2. filtrationThe solid was filtered
  3. washwashed with dichloromethane
  4. washOrganic layer was washed with 10% aqueous solution of NaHCO3 (2×500 mL), water (2×500 mL), brine
  5. customdried
  6. customThe solvent was removed under vacuum