Hydrochloric Acid → Ethyl 2-(2-chloroethylidene)hydrazinecarboxylate

Temperature

30 °C

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.

1. customequipped with a stirrer
2. temperaturethermometer and reflux condenser
3. customThere formed a white crystal slurry
4. stirringAfter further stirring for 15 minutes the mass
5. washThe separated crystals were washed with 30 ml icewater
6. customwere dried in vacuum at room temperture until the weight
7. customThere were obtained white crystals

ORD record

ord-281ca95354bc41ebbed9c39107839dad

Source dataset

uspto-grants-1978_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04113733