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HCID 19012102, Verbindung → HCID 21688812, Verbindung

HRID 1729315
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1729315
[CH3:1][N:2]1[C:7]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][O:17][C:18]3[CH:23]=[CH:22][C:21]([S:24][CH3:25])=[CH:20][C:19]=3[N+:26]([O-])=O)[CH2:10][CH2:9]2)=[CH:6][C:5](=[O:29])[N:4]([CH3:30])[C:3]1=[O:31]>C(O)C>[CH3:1][N:2]1[C:7]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][O:17][C:18]3[CH:23]=[CH:22][C:21]([S:24][CH3:25])=[CH:20][C:19]=3[NH2:26])[CH2:10][CH2:9]2)=[CH:6][C:5](=[O:29])[N:4]([CH3:30])[C:3]1=[O:31]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 19012102HCID 19012102, Verbindung

Produkt 1

HCID 21688812HCID 21688812, VerbindungAusbeute 33,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

2.0 g of the Compound v obtained in Reference Example 17 was dissolved in 20 ml of ethanol, and 4.5 g of stannic chloride (II) was added dropwise. The solution was heated up to 70° C. and then stirred for 30 minutes. The precipitated insolubles were removed by filtration, and the filtrate was then diluted with 100 ml of chloroform. Next, 20 ml of a 1N aqueous sodium hydroxide solution was added to the solution, followed by stirring vigorously. The formed insolubles were removed by filtration, and the resultant chloroform layer was separated, washed with water, dried over anhydrous sodium sulfate and then concentrated. The thus obtained oily product was purified through a silica gel column chromatograph (chloroform/methanol=100/1 in volume ratio), thereby obtaining 0.62 g of 1,3-dimethyl-6-[4-(3-[2-amino-4-methylmercaptophenoxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione (Compound 114).

Aufarbeitung

  1. customThe precipitated insolubles were removed by filtration
  2. additionthe filtrate was then diluted with 100 ml of chloroform
  3. additionNext, 20 ml of a 1N aqueous sodium hydroxide solution was added to the solution
  4. stirringby stirring vigorously
  5. customThe formed insolubles were removed by filtration
  6. customthe resultant chloroform layer was separated
  7. washwashed with water
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated
  10. customThe thus obtained oily product was purified through a silica gel column chromatograph (chloroform/methanol=100/1 in volume ratio)

Quellen und Nachweise

ORD-Eintrag
ord-e1fd41f564104f3d9522d4ab01e8de6d
Quelldatensatz
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05332739

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