Reaction equation
[Cl-].[Zn+2:2].[Cl-].[CH2:4]([NH:10][C:11](=[S:13])[S-:12])[CH2:5][NH:6][C:7](=[S:9])[S-:8].[Na+].[Na+].[CH3:16][N:17]([CH3:21])[C:18](=[S:20])[S-:19].[Na+].Cl.CN(C)C>O>[CH2:4]([NH:10][C:11](=[S:12])[SH:13])[CH2:5][NH:6][C:7](=[S:8])[SH:9].[Zn+2:2].[CH3:16][NH+:17]([CH3:21])[CH3:18].[CH3:16][N:17]([CH3:21])[C:18](=[S:19])[SH:20]Participants
Procedure
A 100 ml. aqueous solution of 6.95g. (0.05 mole) of zinc chloride is added dropwise to a 3-necked flask containing 50 ml. of water. After 5-10 ml. of the solution has been added, a combined 100 ml. aqueous solution of 6.5g. (0.025 mole) of sodium ethylene-bis-dithiocarbamate, 8.95g. (0.05 mole) of sodium dimethyldithiocarbamate and 9.6g. (0.1 mole) of trimethylamine hydrochloride is added to the flask at the same rate as that of the metal salt solution. After the addition, the suspension is stirred 0.5 hour then filtered under vacuum, reslurried with water and filtered again. The collected precipitate is air-dried overnight then dried under vacuum at 45° until it reaches a constant weight. A total of 14.6g. of product, mp 134°-137° C is obtained.
Workup
- additioncontaining 50 ml
- additionof the solution has been added
- additionAfter the addition
- filtrationthen filtered under vacuum
- filtrationfiltered again
- customThe collected precipitate is air-dried overnight
- customthen dried under vacuum at 45° until it
- customof product, mp 134°-137° C is obtained
Sources & evidence
- ORD record
- ord-facce59b8c86404b8cb2f20ce17544a9
- Source dataset
- uspto-grants-1978_03
- Patent number
- US04079146
Linked notes
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