Hexamethylphosphorous triamide → HCID 178420726, Verbindung

HRID 259489

Reaktionsgleichung

Reaktionsgleichung von HRID 259489
CN(C)[P:3](N(C)C)N(C)C.[NH:11]1[CH2:24][CH2:23][CH2:22][NH:21][CH2:20][CH2:19][NH:18][CH2:17][CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1>C1(C)C=CC=CC=1>[N:11]12[PH:3]34[N:18]([CH2:19][CH2:20][N:21]3[CH2:22][CH2:23][CH2:24]1)[CH2:17][CH2:16][CH2:15][N:14]4[CH2:13][CH2:12]2

Komponenten

4

Edukt 2

HCID 15355Hexamethylphosphorous triamideHCID 649641,4,8,11-Tetraazacyclotetradecane

Produkt 1

HCID 178420726HCID 178420726, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A stirred mixture of 4.90 g (30 mmol) of hexamethylphosphorous triamide, 6.00 g (30 mmol) of 1,4,8,11-tetraazacyclotetradecane, and 30 ml of dry toluene is heated to 80°-90°, under nitrogen for 16 hr, then refluxed for 8 hr. The hot solution is filtered under N2 and concentrated, and the residue is sublimed at 60°-70° (0.3 mm) to give 5.45 g (80%) of waxy, white solid 1,4,8,11-tetraaza-15-phosphatetracyclo[6.6.1.04,15.011,15 ]pentadecane.

Aufarbeitung

  1. temperatureis heated to 80°-90°, under nitrogen for 16 hr
  2. temperaturerefluxed for 8 hr
  3. filtrationThe hot solution is filtered under N2
  4. concentrationconcentrated
  5. customis sublimed at 60°-70°

Quellen und Nachweise

ORD-Eintrag
ord-69d32aa3fd2b4bdab2e84ec09634065b
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04038312

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