Dimethyl Sulfate → HCID 54506264, compound
Reaction equation
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]1[NH:10][N:9]([CH3:11])[C:8](=[S:12])[S:7]1.S(OC)(O[CH3:17])(=O)=O.[K]>C(O)C>[CH:6](=[N:10][N:9]([CH3:11])[C:8]([S:7][CH3:17])=[S:12])[C:2]1[O:1][CH:5]=[CH:4][CH:3]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
1 g of 2-(2-furyl)-4-methyl-1,3,4-thidiazolidine-5-thione was dissolved in 50 ml of warm ethanol, and after cooling to room temperature 1.26 g of dimethyl sulphate was added. After stirring for 2.5 hours at 50°, 0.69 g potassium was added, the mixture was heated for 1.5 hours at 50°, then allowed to stand overnight. The reaction mixture was filtered and the filtrate was evaporated to dryness. The residue was recrystallised from ethanol and pure S-methyl 3-furfurylidene- 2-methyl-dithiocarbazate (mp = 103°) was obtained.
Workup
- additionwas added
- temperaturethe mixture was heated for 1.5 hours at 50°
- waitto stand overnight
- filtrationThe reaction mixture was filtered
- customthe filtrate was evaporated to dryness
- customThe residue was recrystallised from ethanol
Sources & evidence
- ORD record
- ord-b87d8b3558254985bd1d8dcd23e21064
- Source dataset
- uspto-grants-1977_12
- Patent number
- US04064262
Reaction notes
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