반응 #1740886

ord-c656649d25e04cfcac9821b911595424

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05403845uspto-grants-1995_04