Potassium Carbonate → HCID 178525644, compound
Reaction equation
[SH:1][C:2]1[S:3][C:4]([SH:7])=[N:5][N:6]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:15][CH2:16][C:17]([OH:19])=[O:18]>CN(C)C=O>[SH:7][C:4]1[S:3][C:2]([S:1][CH2:15][CH2:16][C:17]([OH:19])=[O:18])=[N:6][N:5]=1Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
To a mixture of 1.5 g of 2,5-dimercapto-1,3,4-thiadiazole, 1.3 g of anhydrous potassium carbonate, and 20 ml of N,N-dimethylformamide was added 1.6 g of 3-bromopropionic acid, whereby the red color of the reaction mixture began to gradually fade and the reaction mixture became yellow. Then, the reaction mixture was poured into 100 ml of ice water and extracted with 30 ml of ethyl acetate three times. The extract thus obtained was washed with water and extracted with 20 ml of an aqueous solution of 5% sodium hydrogen carbonate two times. The extract was washed with ethyl acetate, acidified with diluted hydrochloric acid, and extracted with 30 ml of ethyl acetate three times and the extract thus obtained was washed with water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to provide 0.76 g of 3-[(5-mercapto-1,3,4-thiadiazol-2-yl)thio]propionic acid.
Workup
- extractionextracted with 30 ml of ethyl acetate three times
- extractionThe extract thus
- customobtained
- washwas washed with water
- extractionextracted with 20 ml of an aqueous solution of 5% sodium hydrogen carbonate two times
- washThe extract was washed with ethyl acetate
- extractionextracted with 30 ml of ethyl acetate three times
- extractionthe extract thus
- customobtained
- washwas washed with water
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
Sources & evidence
- ORD record
- ord-d3bfbbea58c34e069872f2a0f19b3d0c
- Source dataset
- uspto-grants-1989_08
- Patent number
- US04855310
Reaction notes
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