反应 #3075228
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04144240
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Sodium methoxide (5.4 g., 0.1 mole) and 4-(p-methoxybenzyl)thiosemicarbazide (2.1 g., 0.1 mole) were stirred in methanol (200 ml.) for a period of five minutes. Ethyl oxamate (11.7 g., 0.1 mole) was then added to the mixture and the resulting mixture was refluxed for a period of three hours. At this point, most of the solvent was evaporated under reduced pressure, water (200 ml.) was added to the residue and the pH adjusted to 2.0 with dilute hydrochloric acid. The resulting solid was then filtered and subsequently dried in vacuo at 50° C. to yield pure 1-oxamoyl-4-(p-methoxybenzyl)-3-thiosemicarbazide (25.7 g., 91% yield), m.p. 185°-190° C. the resulting mixture was refluxed for a period of three hours At this point, most of the solvent was evaporated under reduced pressure, water (200 ml.) was added to the residue The resulting solid was then filtered subsequently dried in vacuo at 50° C.
来源 ID: ord-e74cf124327a4d6182c29a75f43dded9