HRID1458363

反应详情

EQUATION

反应方程式

HRID 1458363 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methylmagnesium bromide (0.75 mL of a 3M solution (diethyl ether) in 3.5 mL dry tetrahydrofuran) at 0° C. was added a solution of 4-pyridin-3-yl-butyraldehyde (133 mg in 1 mL tetrahydrofuran) and the mixture at low temperature. After 30 minutes, the reaction was quenched by the addition of saturated ammonium chloride and extracted with ethyl acetate. The organic portion was washed with saturated sodium bicarbonate, dried over sodium sulfate and concentrated in vacuo. Purification by flash chromatography on silica gel (methylene chloride:methanol, 95:5) gave the title compound (71 mg).

WORKUP

后处理

  1. customthe reaction was quenched by the addition of saturated ammonium chloride
  2. extractionextracted with ethyl acetate
  3. washThe organic portion was washed with saturated sodium bicarbonate
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customPurification by flash chromatography on silica gel (methylene chloride:methanol, 95:5)