Triethylamine → HCID 20539557, Verbindung

HRID 1065633

Reaktionsgleichung

Reaktionsgleichung von HRID 1065633
[C:1]1([C:7]2[CH:25]=[CH:24][C:10]([O:11][CH:12]([N:19]3[CH:23]=[N:22][CH:21]=[N:20]3)[CH:13]([OH:18])[C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:26]([Si:28]([CH2:32][CH3:33])([CH2:30][CH3:31])Cl)[CH3:27].C(N(CC)CC)C>C1COCC1.CN(C)C1C=CN=CC=1>[C:1]1([C:7]2[CH:8]=[CH:9][C:10]([O:11][CH:12]([N:19]3[CH:23]=[N:22][CH:21]=[N:20]3)[CH:13]([O:18][Si:28]([CH2:32][CH3:33])([CH2:30][CH3:31])[CH2:26][CH3:27])[C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:24][CH:25]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 13819ChlorotriethylsilaneHCID 91656Bitertanol

Produkt 1

HCID 20539557HCID 20539557, VerbindungAusbeute 40,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

5.5 g of 1-p-phenylphenoxy-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol is dissolved in 25 ml of THF. 2.9 g of triethylchlorosilane and 0.2 g of 4-dimethylaminopyridine are added under a nitrogen blanket. The mixture is heated to 45° C., and 3.3 g of triethylamine is added in portions. After the mixture has been stirred for 14 hours at from 40° to 50° C. it is cooled to room temperature, undissolved matter is filtered off, and the filtrate is concentrated. The product is further purified either by adding petroleum ether, followed by filtration and concentration, or by gel filtration (SiO2, CHCl3). There is obtained 3 g of 1-p-phenylphenoxy-3,3-dimethyl-2-triethylsiloxy-1-(1,2,4-triazol-1-yl)-butane.

Aufarbeitung

  1. temperatureis cooled to room temperature
  2. filtrationundissolved matter is filtered off
  3. concentrationthe filtrate is concentrated
  4. customThe product is further purified either
  5. additionby adding petroleum ether
  6. filtrationfollowed by filtration and concentration
  7. filtrationby gel filtration (SiO2, CHCl3)

Quellen und Nachweise

ORD-Eintrag
ord-2f9a22956e5947f0a32bdb954971dfd7
Quelldatensatz
uspto-grants-1982_05
Patentnummer
US04330535

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