HRID622448

反应详情

EQUATION

反应方程式

HRID 622448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

27 ml of anhydrous pyridine were added to a mixture of 2.0 g of 1-(t-butoxycarbonyl)-3-pyrrolidone and 992 mg of o-methylhydroxylamine hydrochloride, and the mixture was kept stirred overnight at room temperature. After completion of the reaction, the solvent was distilled off and saturated aqueous sodium bicarbonate solution was added to the residue until it was basic. The mixture was extracted with chloroform, and the extract was dried over anhydrous magnesium sulfate and concentrated. The residue was chromatographed over silica gel, using a 3/1 mixture of benzene and ethyl acetate as eluent, giving 2.3 g of 1-(t-butoxycarbonyl)-3-methoxyiminopyrrolidine as a mixture of syn- and anti-isomers.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off
  3. additionsaturated aqueous sodium bicarbonate solution was added to the residue until it
  4. extractionThe mixture was extracted with chloroform
  5. dry with materialthe extract was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was chromatographed over silica gel
  8. additiona 3/1 mixture of benzene and ethyl acetate as eluent