反応 #1866478
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04136196
反応条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 5.7 g. 2,2-dichloropropionic acid and 2.8 g. potassium carbonate in 40 ml water is added a solution of 6.9 g. phenethylhydrazine hydrochloride and 5.6 g. potassium carbonate in 20 ml water. The mixture is heated with stirring to 90° C., a further solution of 5.6 g. potassium carbonate in 20 ml water is dropped in over 30 minutes and further stirred for 60 minutes at 90° C. Afterwards the still alkaline solution is cooled to ambient temperature, shaken out with ether and acidified with concentrated hydrochloric acid. 2-(phenethylhydrazono)-propionic acid crystallizes out and is recrystallized from toluene. The yield is 3.3 g. (40% of theory); m.p. 74°-76° C. The mixture is heated further stirred for 60 minutes at 90° C Afterwards the still alkaline solution is cooled to ambient temperature 2-(phenethylhydrazono)-propionic acid crystallizes out is recrystallized from toluene
ソース ID: ord-9ff0f9e9bbc2492a8ed7624fbdfde6a2