반응 #1769054

ord-afbf09fa394c45db9eda9391e8260392

반응 방정식

CC(C)O
2-propanol
Cl.O=C(O)C1CN=CNC1
1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride
O=S(Cl)Cl
thionyl chloride
C
charcoal
CC(C)OC(=O)C1CN=CNC1.Cl
crystals
수율 84.0%
CC(C)OC(=O)C1CN=CNC1.Cl
Isopropyl 1,4,5,6-Tetrahydropyrimidine-5-carboxylate Hydrochloride
수율 84.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The resulting mixture was refluxed 24 h
  2. 2
    기타by evaporating unreacted alcohol

실험 절차

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (1.0 g, 6.08 mmol) was suspended in 2-propanol (50 ml) and thionyl chloride (0.76 g, 6.39 mmol) was added dropwise. The resulting mixture was refluxed 24 h. The pink solution was treated with charcoal and then reduced in volume to 15 ml by evaporating unreacted alcohol. By allowing the solution to stand overnight, white crystals (1.08 g, 84%) were obtained in three crops, mp 170° C. 300 MHz nmr confirmed product. Microanalysis calc.: C 46.49, H 7.26, N 13.56, found: C 46.49, H 7.25, N 13.64.

출처

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