反应详情

50 ml of benzene, 1.29 g of mercaptoacetic acid and a catalytic amount of p-toluenesulfonic acid monohydrate were added to 2.27 g of 2-(1,3-benzodioxol-5-yl)-2-butanol (crude oil). The obtained mixture was heated under reflux for 11 hours and cooled, followed by the addition of benzene. The obtained mixture was washed with water, followed by the addition of a 1N aqueous solution of sodium hydroxide. The alkaline layer was separated, washed with ethyl acetate, acidified with concentrated hydrochloric acid and extrated with chloroform. The organic layer was washed with water, dried over anhydrous magnesium sulfate and filtered. The filtrate was distilled to remove the solvent. The residue was purified by silica gel column chromatography (chloroform) to obtain 1.11 g of the title compound as a colorless oil.

1. temperatureThe obtained mixture was heated
2. temperatureunder reflux for 11 hours
3. temperaturecooled
4. washThe obtained mixture was washed with water
5. additionfollowed by the addition of a 1N aqueous solution of sodium hydroxide
6. customThe alkaline layer was separated
7. washwashed with ethyl acetate
8. washThe organic layer was washed with water
9. dry with materialdried over anhydrous magnesium sulfate
10. filtrationfiltered
11. distillationThe filtrate was distilled
12. customto remove the solvent
13. customThe residue was purified by silica gel column chromatography (chloroform)