反应详情

In a sealed tube, dissolve p-toluenesulfinic acid sodium salt (5.71 g, 32.1 mmol) in DMF (20 mL) and water (10 mL). Add neo-pentyl bromide (6.3 mL, 48 mmol) and tetrabutylammonium iodide (592 mg, 1.60 mmol) and heat the mixture at 145° C. overnight. Cool the reaction to ambient temperature, dilute with water and extract 3 times with EtOAc. Dry over anhydrous Na2SO4 and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (9:1) to give the desired intermediate as a colorless oil (3.3 g, 45%).

1. temperatureCool
2. customthe reaction to ambient temperature
3. extractionextract 3 times with EtOAc
4. dry with materialDry over anhydrous Na2SO4
5. concentrationconcentrate in vacuo
6. customPurify by chromatography on silica gel eluting with hexane/EtOAc (9:1)