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B Preparation of Semicarbazones and Thiosem
Phthaloyl Cleavage of NPhthaloyl Amino
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2-phthalimido-3-methylbutanal 2-phthalimido-4-methylpentanal 2-phthalimidopropanal acid chloride acidified with dilute alanine amino acids amino group amino-as-triazine Anal aqueous solution as-triazines bath at 100 benzene Calc'd carbazones catalyst chloride was distilled Chloride.-In a 100 compound was prepared condenser dilute hydrochloric acid dissolved in 50 distilled at reduced ethanol ethanol-water mixture ethyl acetate excess thionyl chloride extracted with ether filter four hours given by Emerson47 heated Hefferren4 hydrate hydrazine hydrochloric acid hydrogen chloride insoluble leucine magnetically stirred methionine mixture was magnetically mixture was warmed mole nitrogen oil bath pH of three phenylalanine phthal phthalic anhydride phthalimido aldehyde phthaloyl groups prepared according product was collected product was recrystallized reaction recrystallization reduced pressure refluxed removal of phthaloyl reported value4 residue was dried round-bottom flask equipped semicarbazone hydrochloride sodium acetate sodium hydroxide soluble solution was acidified solution was added solution was complete steam bath sulfur Synthesis tained thionyl chloride thiosemicarbazone three hours valine Water 50 ml yield