Isopropanol → Tris(2,4-DI-tert-butylphenyl)phosphate

HRID 507722

Reaktionsgleichung

Reaktionsgleichung von HRID 507722
[C:1]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=[CH:7][C:6]=1[O:15][P:16]([O:32][C:33]1[CH:38]=[CH:37][C:36]([C:39]([CH3:42])([CH3:41])[CH3:40])=[CH:35][C:34]=1[C:43]([CH3:46])([CH3:45])[CH3:44])[O:17][C:18]1[CH:23]=[CH:22][C:21]([C:24]([CH3:27])([CH3:26])[CH3:25])=[CH:20][C:19]=1[C:28]([CH3:31])([CH3:30])[CH3:29])([CH3:4])([CH3:3])[CH3:2].C([OH:50])(C)C>O>[C:1]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:12])[CH3:13])[CH:8]=[CH:7][C:6]=1[O:15][P:16]([O:32][C:33]1[CH:38]=[CH:37][C:36]([C:39]([CH3:42])([CH3:41])[CH3:40])=[CH:35][C:34]=1[C:43]([CH3:46])([CH3:45])[CH3:44])([O:17][C:18]1[CH:23]=[CH:22][C:21]([C:24]([CH3:25])([CH3:26])[CH3:27])=[CH:20][C:19]=1[C:28]([CH3:31])([CH3:30])[CH3:29])=[O:50])([CH3:2])([CH3:3])[CH3:4]

Komponenten

4

Edukt 2

HCID 3776IsopropanolHCID 91601Tris(2,4-di-tert-butylphenyl) phosphite

Produkt 1

HCID 14572930Tris(2,4-DI-tert-butylphenyl)phosphate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
57.5 °C

Versuchsvorschrift

tris(2,4-Di-tert.butylphenyl)phosphite (5146 g; Irgafos® 168, Ciba Specialty Chemicals) and isopropanol (IPA, 7890 g) are mixed in a reaction vessel and heated to 55-60° C. At this point the mixture is a slurry of approximately 39.0% solids. The peroxide (549 g, 50 weight-% solution of H2O2 in water, 1 equivalent) is added for 2-3 hours while maintaining the pot temperature (reaction is exothermic). After the peroxide addition, the mixture is maintained for 1 hour at 60° C. The reaction mass is homogeneous and the completeness of reaction is checked by LC (>97.0% conversion). Water (1355 g) is added, and the reaction mass is seeded to induce crystallization. Cooling slowly in 2 steps to 45° C. and then to 20° C. completes crystallization. The product is filtered (25μ screen), then dried at 70° C. under full vacuum with a nitrogen sweep.

Aufarbeitung

  1. temperaturewhile maintaining
  2. customthe pot temperature (reaction is exothermic)
  3. temperaturethe mixture is maintained for 1 hour at 60° C
  4. customthe completeness of reaction
  5. customcrystallization
  6. temperatureCooling slowly in 2 steps to 45° C.
  7. customto 20° C.
  8. customcrystallization
  9. filtrationThe product is filtered (25μ screen)
  10. customdried at 70° C. under full vacuum with a nitrogen sweep

Quellen und Nachweise

ORD-Eintrag
ord-56e34206602e4b4e8d3e1d57e57be77b
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786199B2

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