Ammonia → 2,2,2-Trichloroethyl carbamothioylcarbamate
Reaction equation
[S-:1][C:2]#[N:3].[K+].Cl[C:6]([O:8][CH2:9][C:10]([Cl:13])([Cl:12])[Cl:11])=[O:7].[NH3:14]>C(OCC)(=O)C>[C:2]([NH:14][C:6](=[O:7])[O:8][CH2:9][C:10]([Cl:13])([Cl:12])[Cl:11])(=[S:1])[NH2:3]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 60 °C
Procedure
Into 75 ml of dry ethyl acetate, were added 7.3 g of anhydrous potassium thiocyanate and 15.7 g of 2,2,2-trichloroethyl chloroformate. The mixture was stirred at 60° C. for 1.5 hours. The reaction mixture was cooled in ice water, followed by an addition of an aqueous ammonia solution (29%) to render the reaction mixture alkaline. The solvent was removed under reduced pressure. The residue was treated with a water/methanol mixed solvent and the reaction product was obtained in a powdery form through filtration. It was then washed thoroughly with water to obtain 14.5 g of 2,2,2-trichloroethyl N-thiocarbamoylcarbamate.
Workup
- customThe solvent was removed under reduced pressure
- additionThe residue was treated with a water/methanol mixed solvent
- customthe reaction product was obtained in a powdery form through filtration
- washIt was then washed thoroughly with water
Sources & evidence
- ORD record
- ord-29a912f7c64448eb8552b66f9388abeb
- Source dataset
- uspto-grants-1985_04
- Patent number
- US04511574
Reaction notes
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