Acetonitrile → HCID 86694393, Verbindung

HRID 535407Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 535407
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)[N:3]=1.[I:15]N1C(=O)CCC1=O.C(#N)C.S([O-])([O-])(=O)=S.[Na+].[Na+]>C(Cl)Cl>[I:15][C:7]1[C:2]([CH3:1])=[N:3][C:4]([N:9]2[CH2:10][CH2:11][O:12][CH2:13][CH2:14]2)=[N:5][C:6]=1[CH3:8]

Komponenten

6

Edukt 4

HCID 6342AcetonitrileHCID 24477Sodium ThiosulfateHCID 120273N-IodosuccinimideHCID 6768024-(4,6-Dimethylpyrimidin-2-yl)morpholine

Produkt 1

HCID 86694393HCID 86694393, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 4-(4,6-dimethylpyrimidin-2-yl)morpholine (20.6 g, 107 mmol), N-iodosuccinimide (28.8 g, 128 mmol) and ACN (400 ml) is stirred at RT for 24 h. DCM and an aqueous solution containing 3% sodium thiosulfate is added and the mixture extracted with DCM. The combined organic layers are dried over MgSO4 and concentrated in vacuo. This material is used without further purification. Yield: 33.7 g (89%).

Aufarbeitung

  1. additionis added
  2. extractionthe mixture extracted with DCM
  3. dry with materialThe combined organic layers are dried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThis material is used without further purification

Quellen und Nachweise

ORD-Eintrag
ord-6420caeee7c14e74a362fafa8a28f33f
Quelldatensatz
uspto-grants-2014_10
Patentnummer
US08859541B2

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