HRID378576

反应详情

EQUATION

反应方程式

HRID 378576 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice cooled solution of 3.69 g of 4-amino-3,3-dimethyl-1-[1-(R)-phenylethyl]-pyrrolidine in 40 ml of anhydrous tetrahydrofuran there was added 4.92 g of 2-(tert-butoxycarbonylamino)-2-phenylacetonitrile and the mixture was stirred at room temperature for 1 hr. Solvent was removed under reduced pressure, and to the residue there was added ethyl acetate. The mixture was washed with a 1N sodium hydroxide aqueous solution three times and then dried. Solvent was then removed under reduced pressure. The residue was purified through column chromatography using 200 g of silica gel in a column with chloroform as the eluant containing from 1% to 5% methanol to yield 4.32 g of the titled compound.

WORKUP

后处理

  1. customSolvent was removed under reduced pressure
  2. additionto the residue there was added ethyl acetate
  3. washThe mixture was washed with a 1N sodium hydroxide aqueous solution three times
  4. customdried
  5. customSolvent was then removed under reduced pressure
  6. customThe residue was purified through column chromatography
  7. additioncontaining from 1% to 5% methanol