تفاعل #1740886

ord-c656649d25e04cfcac9821b911595424

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe solution was refluxed for 22h
  2. 2
    أخرىThe solvent was evaporated in vacuo to dryness
  3. 3
    أخرىThe residue was crystallized from methanol/THF

الإجراء التجريبي

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (1.5 g, 9.1 mmol) was dissolved in 1-propanol (30 ml). To the mixture was added thionyl chloride (1.1 g, 9.1 mmol) and the solution was refluxed for 22h. The solvent was evaporated in vacuo to dryness. The residue was crystallized from methanol/THF to give 1.06 g (56%) of white crystals, mp 128°-130° C. 300 MHz nmr indicated product. Microanalysis calc.: C 46.49, H 7.26, N 13.56, found: C 46.21, H 6.96, N 17.41.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05403845uspto-grants-1995_04