反应详情

A suspension of 6.0 g of 5-chloromethyl-6-methyl-1,3-benzodioxole, 6.0 g of mercaptoacetic acid and 6.5 g of sodium hydroxide in 130 ml of 50% aqueous ethanol was heated under reflux for one hour and concentrated, followed by the addition of water. The mixture was washed with ethyl acetate. The aqueous layer was acidified with 1N hydrochloric acid and extracted with chloroform. The organic layer was dried over magnesium sulfate and distilled to remove the solvent. The residue was chromatographed over a silica gel column and eluted with chloroform to obtain a crude crystal. This crude crystal was recrystallized from diisopropyl ether to obtain 1.6 g of the title compound as a colorless crystal.

1. temperaturewas heated
2. temperatureunder reflux for one hour
3. concentrationconcentrated
4. additionfollowed by the addition of water
5. washThe mixture was washed with ethyl acetate
6. extractionextracted with chloroform
7. dry with materialThe organic layer was dried over magnesium sulfate
8. distillationdistilled
9. customto remove the solvent
10. customThe residue was chromatographed over a silica gel column
11. washeluted with chloroform
12. customto obtain a crude crystal
13. customThis crude crystal was recrystallized from diisopropyl ether