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

HRID 1653704

反応式

HRID 1653704 の反応式
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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-c656649d25e04cfcac9821b911595424
出典データセット
uspto-grants-1995_04
特許番号
US05403845

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