Chloroacetaldehyde → Ethyl 2-(2-chloroethylidene)hydrazinecarboxylate
Reaction equation
[Cl:1][CH2:2][CH:3]=O.O=[Si]=O.[CH2:8]([O:10][C:11]([NH:13][NH2:14])=[O:12])[CH3:9]>O>[CH2:8]([O:10][C:11](=[O:12])[NH:13][N:14]=[CH:3][CH2:2][Cl:1])[CH3:9]Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
550 g (3.5 mol) of a 50% aqueous solution of chloroacetaldehyde were diluted with 3000 ml water and were reacted with 10 g Celite 545 in order to react with the precipitating resin. For this purpose the solution was passed through a fluted filter into a three times tubulated round bottom flask of 6 l contents which was provided with a stirrer and thermometer. While cooling with ice a solution of 364 g (3.5 mol) of hydrazinoformicacid ethylester in 360 ml water was added during a period of 15 min. The temperature within the reaction vessel was maintained at between 0° and 5° C. There formed immediately a thick white crystal slurry. Stirring was continued at room temperature for 30 minutes. The crystals were then removed by suction, were washed neutral with about 6 liters water and were dried in a vacuum at 30° C. until the weight remained constant.
Workup
- customto react with the precipitating resin
- filtrationa fluted filter into a three times
- customwas provided with a stirrer
- additionwas added during a period of 15 min
- temperatureThe temperature within the reaction vessel was maintained at between 0° and 5° C
- customThere formed immediately a thick white crystal slurry
- customThe crystals were then removed by suction
- washwere washed neutral with about 6 liters water
- customwere dried in a vacuum at 30° C. until the weight
Sources & evidence
- ORD record
- ord-27c7d880a2d44fb58712962039f37116
- Source dataset
- uspto-grants-1978_09
- Patent number
- US04113733
Reaction notes
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