Phosgene → HCID 22125063, Verbindung

HRID 1858191Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1858191
[C:1]([NH:5][CH2:6][C:7]1[C:8]([NH:15][CH3:16])=[N:9][C:10]([S:13][CH3:14])=[N:11][CH:12]=1)([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:24](Cl)(Cl)=[O:25].[Cl-].[NH4+]>O1CCCC1>[C:1]([N:5]1[CH2:6][C:7]2[C:8](=[N:9][C:10]([S:13][CH3:14])=[N:11][CH:12]=2)[N:15]([CH3:16])[C:24]1=[O:25])([CH3:4])([CH3:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 6371PhosgeneHCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 22125127HCID 22125127, Verbindung

Produkt 1

HCID 22125063HCID 22125063, VerbindungAusbeute 83 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel3×

Versuchsvorschrift

A mixture of 240 mg (1 mmol) of 5-tert.butylaminomethyl-4-methylamino-2-methylthiopyrimidine and 0.28 ml of triethylamine in 5 ml of tetrahydrofuran was added dropwise to an ice-cooled solution of 1 ml (1.92 mmol) of phosgene (20% solution in toluene) in 5 ml of tetrahydrofuran. After 1 hour 30 ml of saturated aqueous ammonium chloride and 20 ml of tetrahydrofuran were added to the resulting mixture. The phases were separated. The organic phase was dried over magnesium sulfate, filtered and then evaporated to give 220 mg (83%) of 3-tert.butyl-7-methylthio-3,4-dihydro-1-methylpyrimido[4,5-d]pyrimidin-2(1H)-one as a white solid.

Aufarbeitung

  1. customThe phases were separated
  2. dry with materialThe organic phase was dried over magnesium sulfate
  3. filtrationfiltered
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-f19d01b856634e6284350401e22e247d
Quelldatensatz
uspto-grants-2000_11
Patentnummer
US06150373

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