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Stearoyl chloride → HCID 20249612, Verbindung

HRID 1077116
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1077116
[OH:1][CH2:2][C:3]12[CH2:10][O:9][P:6]([O:7][CH2:8]1)[O:5][CH2:4]2.[C:11](Cl)(=[O:29])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].C(N(CC)CC)C>C1(C)C=CC=CC=1>[P:6]12[O:9][CH2:10][C:3]([CH2:2][O:1][C:11](=[O:29])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])([CH2:8][O:7]1)[CH2:4][O:5]2
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Komponenten

5

Edukt 3

HCID 8212Stearoyl chlorideHCID 8471TriethylamineHCID 200183Pentaerythritol phosphite

Produkt 1

HCID 20249612HCID 20249612, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

16.4 g (0.1 mol) of 4-hydroxymethyl-1-phospha-2,6,7-trioxabicyclo[2,2,2]octane are dissolved in 150 ml of toluene by warming. 30.2 g (0.1 mol) of stearic acid chloride, followed by 10.1 g (0.1 mol) of triethylamine, are added dropwise at room temperature. After the slight evolution of heat has died away, the mixture is stirred for 10 hours under nitrogen at room temperature and the precipitated triethylamine hydrochloride is then filtered off. The filtrate is evaporated with exclusion of moisture, a yellowish oil remaining, which crystallises on being triturated with methanol. After filtering off under suction and drying, stearic acid 1-phospha-2,6,7-trioxabicyclo[2,2,2]oct-4-yl-methyl ester (Stabiliser No. 9), melting point 49°C, is obtained.

Aufarbeitung

  1. temperatureby warming
  2. additionare added dropwise at room temperature
  3. temperatureAfter the slight evolution of heat
  4. filtrationthe precipitated triethylamine hydrochloride is then filtered off
  5. customThe filtrate is evaporated with exclusion of moisture
  6. customwhich crystallises
  7. customon being triturated with methanol
  8. filtrationAfter filtering off under suction
  9. customdrying

Quellen und Nachweise

ORD-Eintrag
ord-c2a9fb2568c74e0e9c13a88c9bb1392a
Quelldatensatz
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03959413

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