1-Propanol → n-Propyl 1,4,5,6-Tetrahydropyrimidine-5-carboxylate Hydrochloride

HRID 1653704

반응식

HRID 1653704 반응식
Cl.[NH:2]1[CH2:7][CH:6]([C:8]([OH:10])=[O:9])[CH2:5][N:4]=[CH:3]1.S(Cl)([Cl:13])=O.[CH2:15](O)[CH2:16][CH3:17]>>[ClH:13].[NH:4]1[CH2:5][CH:6]([C:8]([O:10][CH2:15][CH2:16][CH3:17])=[O:9])[CH2:7][N:2]=[CH:3]1

참가 물질

4

반응물 3

HCID 10311-PropanolHCID 24386Thionyl ChlorideHCID 703421841,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride

생성물 1

HCID 45261147n-Propyl 1,4,5,6-Tetrahydropyrimidine-5-carboxylate Hydrochloride수율 56%

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.

후처리

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

출처 및 근거

ORD 기록
ord-c656649d25e04cfcac9821b911595424
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05403845

연결된 노트

불러오는 중…