Pentachlorophenol → HCID 131710245, Verbindung

HRID 1076838Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1076838
[CH3:1][O:2][C@H:3]1[O:8][C@H:7]([CH2:9][OH:10])[C@@H:6]([OH:11])[C@H:5]([OH:12])[C@H:4]1[OH:13].[Cl:14][C:15]1[C:20]([OH:21])=[C:19]([Cl:22])[C:18]([Cl:23])=[C:17]([Cl:24])[C:16]=1[Cl:25].[Al].[CH2:27]([O:29][P:30]([O:34][CH2:35][CH3:36])[O:31][CH2:32][CH3:33])[CH3:28].[CH2:37]1[O:40][CH:38]1[CH3:39]>[Fe].C(N(CC)CC)C>[CH3:1][O:2][C@H:3]1[O:8][C@H:7]([CH2:9][OH:10])[C@@H:6]([OH:11])[C@H:5]([OH:12])[C@H:4]1[OH:13].[CH2:27]([O:29][P:30]([O:34][CH2:35][CH3:36])[O:31][CH2:32][CH3:33])[CH3:28].[Cl:14][C:15]1[C:20]([OH:21])=[C:19]([Cl:22])[C:18]([Cl:23])=[C:17]([Cl:24])[C:16]=1[Cl:25].[CH2:37]1[O:40][CH:38]1[CH3:39]

Komponenten

8

Edukt 5

HCID 992PentachlorophenolHCID 6378Propylene Oxide2×HCID 31215Triethyl phosphiteHCID 64947methyl alpha-D-glucopyranosideHCID 5359268Aluminum

Produkt 1

HCID 131710245HCID 131710245, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 8471TriethylamineLösungsmittel

Reaktionsbedingungen

Temperatur
122 °C

Versuchsvorschrift

A 5-liter flask, standardly equipped, was charged with 776 grams of alpha-methylglucoside, 1264 grams of pentachlorophenol containing about 750 ppm of aluminum and iron compounds, 240 grams of triethylphosphite, and heated to 122°C. 1025 ml. of propylene oxide was added at 122°-138°C. over a 6-hour period. Then 48 grams of triethylamine was added, followed by 265 ml. more of propylene oxide to reduce the acid number to less than 1. The mixture was then stripped for 2 hours at 80°-85°C/2 mm. Hg to remove volatiles. The oxypropylated product weighed 3827 grams and analyzed as follows:

Aufarbeitung

  1. customA 5-liter flask, standardly equipped
  2. custom/2 mm. Hg to remove volatiles

Quellen und Nachweise

ORD-Eintrag
ord-5023106919ff4622976632ee697b3ffb
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03957922

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