ethyl N-(2-chloroethylideneamino)carbamate

Conditions: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 60 ml water and 0.8 ml of concentrated hydrochloric acid were heated to 90° C. in a three times tubulated round bottom flask of 250 ml contents equipped with a stirrer, thermometer and reflux condenser. The reaction mass was then reacted with 15.2 g of chloroacetaldehydediethylacetal and was subjected to stirring for 15 minutes at 90° to 100° C. The mass was then cooled to 30° C. and a solution of 12.5 g of hydrazinoformic acid ethylester in 40 ml water was added within a period of 10 minutes. There formed a white crystal slurry. After further stirring for 15 minutes the mass was subjected to suction. The separated crystals were washed with 30 ml icewater and were dried in vacuum at room temperture until the weight remained constant. There were obtained white crystals. equipped with a stirrer thermometer and reflux condenser There formed a white crystal slurry After further stirring for 15 minutes the mass The separated crystals were washed with 30 ml icewater were dried in vacuum at room temperture until the weight There were obtained white crystals

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

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. to react with the precipitating resin a fluted filter into a three times was provided with a stirrer 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 The crystals were then removed by suction were washed neutral with about 6 liters water were dried in a vacuum at 30° C. until the weight