Реакция #1769055

ord-a713f6be2aa04ac2bddbc2d06f5e6cef

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеprecipitation
  2. 2
    ДругоеThe white solids were collected
  3. 3
    Другоеcrystallized from methanol/THF

Методика

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (1.0 g, 6.1 mmol) was suspended in dry benzyl alcohol (20 ml). To the mixture was added thionyl chloride (0.76 g, 6.39 mmol) and the resulting mixture was heated in an oil bath at 80° C. for 24 h. The clear solution was poured to anhydrous ethyl ether (100 ml) to induce precipitation. The white solids were collected and crystallized from methanol/THF to give 1.18 g (76%) of product (mp 113°-114° C.). 300 MHz nmr indicated the product. Microanalysis calc.: C 56.58, H 5.89, N 11.00; found: C 56.34, H 6.03, N 11.19.

Источник

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