Hydrochloric Acid → HCID 86745512, compound

(2S,4S)-1-Methyl-2-dimethylaminocarbonyl-4-acetylthiopyrrolidine (660 mg) was dissolved in methanol (6.6 ml), and a solution of sodium methoxide (155 mg) in methanol (2.2 ml) was added thereto at room temperature under nitrogen stream, followed by stirring at the same temperature for 3 minutes. To the reaction mixture, 6N hydrochloric acid (1.05 ml) was added, and the solvent was removed by distillation. The residue was dissolved in ethanol (10.5 ml), and active carbon (99 mg) was added thereto under reflux. After refluxing for 15 minutes, the resultant mixture was filtered while hot, and the filtrate was concentrated under reduced pressure. The residue was dissolved in dichloromethane and dried over magnesium sulfate. Removal of the solvent gave (2S,4S)-1-methyl-2-dimethylaminocarbonyl-4-mercaptopyrrolidine hydrochloride.

1. customat room temperature
2. customthe solvent was removed by distillation
3. dissolutionThe residue was dissolved in ethanol (10.5 ml)
4. additionactive carbon (99 mg) was added
5. temperatureunder reflux
6. temperatureAfter refluxing for 15 minutes
7. filtrationthe resultant mixture was filtered while hot, and the filtrate
8. concentrationwas concentrated under reduced pressure
9. dissolutionThe residue was dissolved in dichloromethane
10. dry with materialdried over magnesium sulfate
11. customRemoval of the solvent

ORD record

ord-a7f5d6da5cbf4cd0b516fae1716e1cd3

Source dataset

uspto-grants-1992_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05093328