Potassium Carbonate → HCID 85518231, compound
Reaction equation
[C:1]([CH:3](C#N)[CH2:4][S:5][CH2:6][CH:7](C#N)[C:8]#[N:9])#[N:2].C(=O)([O-])[O-].[K+].[K+].[Br:20]Br>ClC(Cl)C>[C:1]([CH2:3][CH2:4][S:5][CH:6]=[C:7]([Br:20])[C:8]#[N:9])#[N:2]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 40 °C
Procedure
28 g of bis-cyanoethyl sulphide were dissolved in 50 ml of dichloroethane, and 110 g of potassium carbonate were added. 64 g of bromine were then added dropwise at 20° to 30° C. The mixture was stirred at 40° C. for 16 hours, a further 40 g of potassium carbonate were added and the mixture was stirred at 60° C. for 16 hours. The mixture was filtered, the filtrate was washed with water and concentrated and the residue was chromatographed. 5.5 g of 2-bromo-2-cyano-vinyl 2-cyano-ethyl sulphide were obtained as an oil, 1H-NMR: δ=2.6-3.0 (2H), 3.0-3.4 (2H) and 7.5-7.9 (1H).
Workup
- stirringthe mixture was stirred at 60° C. for 16 hours
- filtrationThe mixture was filtered
- washthe filtrate was washed with water
- concentrationconcentrated
- customthe residue was chromatographed
Sources & evidence
- ORD record
- ord-7b237a94b48f419780f04e85b50bc0d4
- Source dataset
- uspto-grants-1987_03
- Patent number
- US04647687
Reaction notes
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