Trilauryl phosphite → Di-n-dodecyl 4-tert.-butyl-2,6-dimethyl-3-hydroxybenzylphosphonate

HRID 1658032

Reaktionsgleichung

Reaktionsgleichung von HRID 1658032
[P:1]([O:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH3:40])([O:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[O:2]CCCCCCCCCCCC.[C:41]([C:45]1[C:50]([OH:51])=[C:49]([CH3:52])[C:48]([CH2:53]Cl)=[C:47]([CH3:55])[CH:46]=1)([CH3:44])([CH3:43])[CH3:42]>>[C:41]([C:45]1[CH:46]=[C:47]([CH3:55])[C:48]([CH2:53][P:1](=[O:2])([O:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[O:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH3:40])=[C:49]([CH3:52])[C:50]=1[OH:51])([CH3:44])([CH3:43])[CH3:42]

Komponenten

3

Edukt 2

HCID 76495Trilauryl phosphiteHCID 901316-tert-Butyl-3-(chloromethyl)-2,4-dimethylphenol

Produkt 1

HCID 21311762Di-n-dodecyl 4-tert.-butyl-2,6-dimethyl-3-hydroxybenzylphosphonate

Versuchsvorschrift

41 Grams of trilauryl phosphite and 16.1 grams of 6-tert.-butyl-3-chloromethyl-2,4-dimethylphenol were stirred together as a melt at 105° to 110° for 1 hour, followed by 110° to 120° for 2 hours, 120° to 125° for 10 hours and finally at 140° to 145° for 4 hours. The crude was topped in the "ASCO 50" Rotafilm Molecular Still at a wall temperature of 80° to 90° at 1 to 5 microns Hg. pressure to remove most of the by-product dodecyl chloride as well as small amounts of other volatiles. This topping procedure was repeated at a wall temperature of 200° to 210° at the same pressure to remove additional volatiles. The desired product distilled at a wall temperature of 250° to 260° at 1 micron Hg. pressure yielding the desired product as a colorless liquid which solidified to a white solid (m.p. 36° to 42°). (compound 3)

Aufarbeitung

  1. customwas topped in the "ASCO 50" Rotafilm Molecular Still at a wall temperature of 80° to 90° at 1 to 5 microns Hg
  2. custompressure to remove most of the by-product dodecyl chloride as well as small amounts of other volatiles
  3. customwas repeated at a wall temperature of 200° to 210° at the same pressure
  4. customto remove additional volatiles
  5. distillationThe desired product distilled at a wall temperature of 250° to 260° at 1 micron Hg

Quellen und Nachweise

ORD-Eintrag
ord-b2e5072362264fe78c0a76b00ab98b7a
Quelldatensatz
uspto-grants-1976_06
Patentnummer
US03962376

Verknüpfte Notizen

Wird geladen…