반응 #1769053

ord-1ef97c7f63eb4aceb16ae05fb905f366

반응 방정식

Cl.O=C(O)C1CN=CNC1
1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride
CCCO
1-propanol
O=S(Cl)Cl
thionyl chloride
CCCOC(=O)C1CN=CNC1.Cl
white crystals
수율 56.0%
CCCOC(=O)C1CN=CNC1.Cl
n-Propyl 1,4,5,6-Tetrahydropyrimidine-5-carboxylate Hydrochloride
수율 56.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the solution was refluxed for 22 h
  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 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05175166uspto-grants-1992_12