Реакция #1769053

ord-1ef97c7f63eb4aceb16ae05fb905f366

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05175166uspto-grants-1992_12