HRID334082

反应详情

EQUATION

反应方程式

HRID 334082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 545 mg (1.78 mmol) [benzyl-(1-cyano-2-methoxy-1-methyl-ethyl)-amino]-acetic acid ethyl ester in 10 mL MeOH was added 460 mg (3.57 mmol) cobalt(II) chloride. The mixture was cooled with ice and 270 mg (7.13 mmol) sodium borohydride was added. The resulting mixture was stirred at RT for 1 h. The reaction mixture was diluted with a small amount of water, acidified with acetic acid and stirred for 30 min. The organic solvent was removed by distillation; the residue was alkalized with 4 N aqueous NaOH solution and filtered through Celite. The solvent was extracted with EtOAc. The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo.

WORKUP

后处理

  1. additionwas added
  2. stirringstirred for 30 min
  3. customThe organic solvent was removed by distillation
  4. filtrationfiltered through Celite
  5. extractionThe solvent was extracted with EtOAc
  6. dry with materialThe combined organic phases were dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo