HRID473441

反应详情

EQUATION

反应方程式

HRID 473441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (S)-tert-butyl 1-(methoxy(methyl)amino)-1-oxopropan-2-ylcarbamate (1.16 g, 5 mmol) in THF (10 mL) was cooled to −15° C. and slowly charged with isopropylmagnesium chloride (2.0M, 2.37 mL, 0.95 eq). After a clear solution was obtained, benzylmagnesium chloride (1.0M, 4.99 mL, 1.0 eq) was added dropwise with stirring at rt overnight. The reaction mixture was quenched with NH4Cl solution and extracted with EtOAc (10 mL×2). The combined organic layers were washed with water, brine, dried over sodium sulfate before being filtered, concentrated to give a white solid as (S)-tert-butyl 3-oxo-4-phenylbutan-2-ylcarbamate. Mass Spectrum (ESI) m/e=264 (M+1).

WORKUP

后处理

  1. customAfter a clear solution was obtained
  2. customThe reaction mixture was quenched with NH4Cl solution
  3. extractionextracted with EtOAc (10 mL×2)
  4. washThe combined organic layers were washed with water, brine
  5. dry with materialdried over sodium sulfate
  6. filtrationbefore being filtered
  7. concentrationconcentrated