Malononitrile → Potassium bromide--dibromopropanedinitrile (1/1/1)
Reaction equation
[C:1](#[N:5])[CH2:2][C:3]#[N:4].[Br-:6].[K+:7].[Br:8]Br>O>[Br:6][C:2]([Br:8])([C:1]#[N:5])[C:3]#[N:4].[Br-:6].[K+:7]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 99 g of malononitrile and 75 g of potassium bromide in 900 ml of water was cooled to 5°-10° and 158 ml of bromine were slowly added at 5°-10° during 21/2 hours. After addition was completed, the mixture was stirred for 2 hours at 5°-10°, then was filtered. The collected solid was washed with 150 ml of ice-water and air-dried on the filter. A second crop was obtained by filtering the filtrate after a short quiescent period. The isolated solids were combined and dried to constant weight in a desiccator over phosphorus pentoxide (the presence of bromine vapors necessitated replenishing the phosphorus pentoxide) to give 337.5 g of the complex, which was used without further purification.
Workup
- temperaturewas cooled to 5°-10°
- additionAfter addition
- filtrationwas filtered
- washThe collected solid was washed with 150 ml of ice-water
- customair-dried on the filter
- customA second crop was obtained
- filtrationby filtering the filtrate after a short quiescent period
- dry with materialdried to constant weight in a desiccator over phosphorus pentoxide (the presence of bromine vapors
Sources & evidence
- ORD record
- ord-dd4899e5a35146cbbcd187b75e22279d
- Source dataset
- uspto-grants-1978_02
- Patent number
- US04075001
Reaction notes
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