Morpholine → 4-(2,6-Dichloro-5-methylsulfanyl-pyrimidin-4-yl)-morpholine

HRID 629007Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 629007
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([S:9][CH3:10])=[C:4](Cl)[N:3]=1.[NH:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1>C1COCC1>[Cl:1][C:2]1[N:3]=[C:4]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[C:5]([S:9][CH3:10])=[C:6]([Cl:8])[N:7]=1

Komponenten

4

Edukt 2

HCID 8083MorpholineHCID 122255442,4,6-Trichloro-5-methylsulfanyl-pyrimidine

Produkt 1

HCID 866734944-(2,6-Dichloro-5-methylsulfanyl-pyrimidin-4-yl)-morpholine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of 2,4,6-trichloro-5-methylsulfanyl-pyrimidine (4.0 g, 17.4 mmol.), morpholine (2.3 g, 26.1 mmol, 1.5 eq.) and THF (20 ml) was stirred at room temperature for 2.0 hr. The reaction mixture was dried and the solvent was evaporated. Thereafter, a 0.1 N HCl washing free morpholine was added to the solution. The solution was extracted with EA and the EA in the solution was removed by evaporation. A crude product was obtained. Purification of the crude by flash chromatography on silica gel (Hexane/EtOAc 6:1) gave a gray solid of 2.34 g (48.2%).

Aufarbeitung

  1. customThe reaction mixture was dried
  2. customthe solvent was evaporated
  3. additionThereafter, a 0.1 N HCl washing free morpholine was added to the solution
  4. extractionThe solution was extracted with EA
  5. customthe EA in the solution was removed by evaporation

Quellen und Nachweise

ORD-Eintrag
ord-9238518658e34504a3ad54387e02e5fa
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09315491B2

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