تفاعل #1769053

ord-1ef97c7f63eb4aceb16ae05fb905f366

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe solution was refluxed for 22 h
  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 22 h. 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: US05175166uspto-grants-1992_12