HRID1577469

反应详情

EQUATION

反应方程式

HRID 1577469 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 200 ml four-necked flask, there were charged α-bromo-tert-butylacetic acid (9.8 g) and benzene (50 ml), and pyridine (50 ml) and α,α-dimethylbenzylamine (6.9 g) were dropwise added thereto while stirring at room temperature. Dicyclohexylcarbodiimide (10.8 g) was further added thereto, and the reaction was continued at 60°-70° C. for 6 hours, followed by cooling. The solvent was distilled off under reduced pressure, and the residue was extracted with hot benzene. The benzene extract was concentrated by distillation, and the residue was recrystallized from ethanol to give N-(α,α-dimethylbenzyl)-α-bromo-tert-butylacetamide (10.8 g).

WORKUP

后处理

  1. additionwere dropwise added
  2. temperatureby cooling
  3. distillationThe solvent was distilled off under reduced pressure
  4. extractionthe residue was extracted with hot benzene
  5. extractionThe benzene extract
  6. concentrationwas concentrated by distillation
  7. customthe residue was recrystallized from ethanol