Acetonitrile → HCID 66802658, Verbindung

HRID 341469

Reaktionsgleichung

Reaktionsgleichung von HRID 341469
[CH2:1]([N:8]([CH3:17])[C:9]1[N:14]=[C:13]([NH2:15])[N:12]=[C:11](Cl)[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:18](#[N:20])C>[C-]#N.C([N+](CCCC)(CCCC)CCCC)CCC.CCOC(C)=O>[NH2:15][C:13]1[N:14]=[C:9]([N:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH3:17])[N:10]=[C:11]([C:18]#[N:20])[N:12]=1

Komponenten

5

Edukt 2

HCID 6342AcetonitrileHCID 568317906-Chloro-N2-methyl-N2-(phenylmethyl)-1,3,5-triazine-2,4-diamine2×

Produkt 1

HCID 66802658HCID 66802658, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 165872Tetrabutylammonium CyanideKatalysatorHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To N-Benzyl-6-chloro-N-methyl-[1,3,5]triazine-2,4-diamine (Intermediate 34, 350 mg, 1.40 mmol) was added tetra n-butylammonium cyanide (1.15 g, 4.28 mmol) and anhydrous acetonitrile (15 mL). The reaction mixture was stirred at 50 C for 1 h, diluted with EtOAc (20 mL), extracted with water (2×10 mL), dried over anhydrous sodium sulfate and concentrated under reduced pressure to furnish the desired product, which was used directly without further purification (327 mg, 97%). Method C HPLC-MS: MH+ requires m/z=241. Found: m/z=241, Rt=1.29 min (86%).

Aufarbeitung

  1. extractionextracted with water (2×10 mL)
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c6704323257b433fa57dc790b9103f38
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08895733B2

Verknüpfte Notizen

Wird geladen…