反应详情

11.9 grams (40.7 mmoles) of 6-acetylthio-8-methylthiooctanoic acid ethyl ester (XI) were added to a solution of 7.5 grams (133.7 mmoles) of potassium hydroxide in 100 ml of methanol and 5 ml of water and the mixture heated at reflux for 10 hours under a cover of nitrogen. After a further 10 hours at room temperature the solvent was removed in a vacuum, the residue taken up on 100 ml of 3N hydrochloric acid and extracted three times, each time with 100 ml of ethyl acetate. After drying the combined extracts with magnesium sulfate the solvent was removed in a vacuum. The short path distillation of the residue gave 7.1 grams (78% of theory) of 6-mercapto-8-methylthiooctanoic acidas a pale yellow oil having a boiling point of 150° C. to 170° C. at 0.5 mbar.

1. temperaturethe mixture heated
2. temperatureat reflux for 10 hours under a cover of nitrogen
3. customAfter a further 10 hours at room temperature the solvent was removed in a vacuum
4. extractionextracted three times
5. dry with materialAfter drying the combined extracts with magnesium sulfate the solvent
6. customwas removed in a vacuum
7. distillationThe short path distillation of the residue
8. customgave 7.1 grams (78% of theory) of 6-mercapto-8-methylthiooctanoic acidas a pale yellow oil