Hydrochloric Acid → 1-(2-Hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione

HRID 256537

Reaktionsgleichung

Reaktionsgleichung von HRID 256537
[NH2:1][CH2:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][OH:8].[C:9](=S)=[S:10].Cl>C(O)C.O>[OH:8][CH2:7][CH2:6][N:5]1[CH2:4][CH2:3][CH2:2][NH:1][C:9]1=[S:10]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 6348Carbon Disulfide3×HCID 78211N-(Aminopropyl)ethanolamine

Produkt 1

HCID 36032811-(2-Hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 19096565Water ethanolLösungsmittel

Versuchsvorschrift

2-(3-Aminopropylamino)ethanol (118 ml) is dissolved in 1:1 ethyl alcohol-water (340 ml) and heated to 40°-50° C. Carbon disulfide (60 ml) is added dropwise over a period of about 15 minutes. An exothermic reaction occurs after about half of the amount of carbon disulfide is added. After the addition of all the carbon disulfide, the mixture is refluxed for about 1 hour. Concentrated hydrochloric acid (8 ml) is then added, and the reaction mixture is refluxed overnight. After cooling in an ice bath, the crystalline solid which separates is filtered, washed with isopropyl alcohol and t-butyl methyl ether, and dried to give 129-4 g of 1-(2-hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione, melting point 112°-114° C.

Aufarbeitung

  1. temperatureheated to 40°-50° C
  2. customAn exothermic reaction
  3. additionis added
  4. temperaturethe mixture is refluxed for about 1 hour
  5. temperaturethe reaction mixture is refluxed overnight
  6. temperatureAfter cooling in an ice bath
  7. filtrationthe crystalline solid which separates is filtered
  8. washwashed with isopropyl alcohol and t-butyl methyl ether
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-4d01249e829942b499b83f7e31d5cabb
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05258381

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