HRID1922701

反应详情

EQUATION

反应方程式

HRID 1922701 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 3.0 M solution of methylmagnesium bromide in Et2O (0.98 mL, 2.92 mmol), at 0° C., was added a solution of 3-oxoazetidine-1-carboxylic acid benzyl ester (0.5 g, 2.44 mmol) in anhydrous THF (5 mL) dropwise over 5 min under argon. The reaction mixture was stirred for 18 h at room temperature, and then quenched by addition of a saturated aqueous solution of NH4Cl (2.5 mL) and water (5 mL). The aqueous phase was extracted with EtOAc (10 mL) The organic layer was separated, dried over sodium sulphate and concentrated in vacuo to give 3-Hydroxy-3-methylazetidine-1-carboxylic acid benzyl ester as a colourless oil (0.54 g, 99%). LCMS (Method A): RT=3.60 min, [M+H]+ 221.9

WORKUP

后处理

  1. customquenched by addition of a saturated aqueous solution of NH4Cl (2.5 mL) and water (5 mL)
  2. extractionThe aqueous phase was extracted with EtOAc (10 mL) The organic layer
  3. customwas separated
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated in vacuo