Toluene → HCID 19738525, Verbindung

HRID 1460795Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1460795
[H-].[Na+].C1(C)C=CC=CC=1.[CH3:10][O:11][CH:12]([O:20][CH3:21])[CH2:13][NH:14][C:15](=[O:19])[O:16][CH2:17][CH3:18].Cl[CH2:23][C:24]([CH2:26][F:27])=[CH2:25]>O>[F:27][CH2:26][C:24](=[CH2:23])[CH2:25][N:14]([CH2:13][CH:12]([O:11][CH3:10])[O:20][CH3:21])[C:15](=[O:19])[O:16][CH2:17][CH3:18]

Komponenten

6

Edukt 4

HCID 1140TolueneHCID 24758Sodium hydrideHCID 10921057Ethyl 2,2-dimethoxyethylcarbamateHCID 140720532-(Chloromethyl)-3-fluoroprop-1-ene

Produkt 1

HCID 19738525HCID 19738525, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

8 g (0.26 mol) of sodium hydride (80% pure) are initially introduced into 200 ml of toluene and 35.8 g (0.2 mol) of ethyl N-(2,2-dimethoxyethyl)-carbamate are added dropwise at 90° C. The mixture is then stirred for one hour at 90° C. and 32.6 g (0.3 mol) of 1-chloro-2-fluoromethylprop-2-ene are then added dropwise. The mixture is stirred overnight at 90° C., salts are dissolved in water, and the aqueous phase is separated off and extracted with toluene. The organic phases are dried over potassium carbonate and concentrated, and the residue is distilled.

Aufarbeitung

  1. additionare added dropwise at 90° C
  2. stirringThe mixture is stirred overnight at 90° C.
  3. customthe aqueous phase is separated off
  4. extractionextracted with toluene
  5. dry with materialThe organic phases are dried over potassium carbonate
  6. concentrationconcentrated
  7. distillationthe residue is distilled

Quellen und Nachweise

ORD-Eintrag
ord-8c0de8319c124181a5ceffadbac46033
Quelldatensatz
uspto-grants-1991_12
Patentnummer
US05071999

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