Water → HCID 57210743, Verbindung

HRID 2231975Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2231975
[Cl:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([Cl:10])[C:5]([Cl:11])=[C:4](Cl)[C:3]=1[Cl:13].NCCNC(=O)[CH:19]([C:21]1[CH:26]=[C:25]([C:27]([CH3:30])([CH3:29])[CH3:28])[C:24]([OH:31])=[C:23]([C:32]([CH3:35])([CH3:34])[CH3:33])[CH:22]=1)[CH3:20].C([N:39](CC)CC)C.O.C[N:46]1[CH2:50][CH2:49]C[C:47]1=[O:51]>C1(C)C=CC=CC=1>[C:32]([C:23]1[CH:22]=[C:21]([CH2:19][CH2:20][C:47]([NH:46][CH2:50][CH2:49][NH:39][C:4]2[C:5]([Cl:11])=[C:6]([Cl:10])[C:7]([C:8]#[N:9])=[C:2]([Cl:1])[C:3]=2[Cl:13])=[O:51])[CH:26]=[C:25]([C:27]([CH3:30])([CH3:28])[CH3:29])[C:24]=1[OH:31])([CH3:35])([CH3:34])[CH3:33]

Komponenten

7

Edukt 5

HCID 962WaterHCID 8471TriethylamineHCID 13387N-methyl-2-pyrrolidoneHCID 30363PentachlorobenzonitrileHCID 22104623HCID 22104623, Verbindung

Produkt 1

HCID 57210743HCID 57210743, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

27.6 g of pentachlorobenzonitrile and 32 g of 3,5-di-tert-butyl-4-hydroxyphenylpropionic acid 2-aminoethylamide are reacted with 11 g of triethylamine in 200 g of N-methylpyrrolidone for 7 hours at 100° C., after which 500 g of water and 400 g of toluene are added, and the toluene phase is separated off while still hot and evaporated down under reduced pressure. The residue is boiled with 0.15 l of ethanol, and the mixture is left to stand overnight at room temperature. The precipitate is then filtered off under suction and dried. After recrystallization from toluene, the product melts at 173°-175° C.

Aufarbeitung

  1. customthe toluene phase is separated off while still hot and
  2. customevaporated down under reduced pressure
  3. waitthe mixture is left
  4. filtrationThe precipitate is then filtered off under suction
  5. customdried
  6. customAfter recrystallization from toluene

Quellen und Nachweise

ORD-Eintrag
ord-fa9c5be00d714278a88effefbf532837
Quelldatensatz
uspto-grants-1988_11
Patentnummer
US04785107

Notizen zur Reaktion

Wird geladen…