3-Amino-1-propanol → HCID 135433506, Verbindung

HRID 363364Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 363364
Cl[C:2]1[CH:7]=[C:6]([OH:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[O:15][CH2:16][CH2:17][CH3:18])[N:3]=1.[NH2:19][CH2:20][CH2:21][CH2:22][OH:23]>C(O)CC>[OH:23][CH2:22][CH2:21][CH2:20][NH:19][C:2]1[N:3]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[O:15][CH2:16][CH2:17][CH3:18])[NH:5][C:6](=[O:8])[CH:7]=1

Komponenten

4

Edukt 2

HCID 90863-Amino-1-propanolHCID 178458304HCID 178458304, Verbindung

Produkt 1

HCID 135433506HCID 135433506, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 10311-PropanolLösungsmittel

Versuchsvorschrift

A stirred solution of 4-chloro-6-hydroxy-2-(2-propoxyphenyl)pyrimidine (0.66 g) and 3-amino-1-propanol (0.56 g) in n-propanol was heated under reflux for 16 hours. The cooled reaction mixture was evaporated under reduced pressure to yield an oil which was partitioned between chloroform (20 ml) and water (20 ml). The chloroform layer was separated from the aqueous layer which was extracted with chloroform (2×10 ml) and the combined chloroform layers were washed with water, dried (magnesium sulfate) and evaporated under reduced pressure. The residue was recrystallized from isopropanol:diethyl ether to yield the title compound, 0.54 g, m.p. 147.5°-148.5° C.

Aufarbeitung

  1. temperatureunder reflux for 16 hours
  2. customThe cooled reaction mixture
  3. customwas evaporated under reduced pressure
  4. customto yield an oil which
  5. customwas partitioned between chloroform (20 ml) and water (20 ml)
  6. customThe chloroform layer was separated from the aqueous layer which
  7. extractionwas extracted with chloroform (2×10 ml)
  8. washthe combined chloroform layers were washed with water
  9. dry with materialdried (magnesium sulfate)
  10. customevaporated under reduced pressure
  11. customThe residue was recrystallized from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-01a017a6fdcc498cab036fb016f8a4dd
Quelldatensatz
uspto-grants-1999_02
Patentnummer
US05874440

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