Triethylamine → 4-Methoxybenzyl(2-methoxyethyl)carbamoyl chloride

HRID 2212962Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2212962
ClC([O:4][C:5]([Cl:8])(Cl)Cl)=O.[CH3:9][O:10][C:11]1[CH:22]=[CH:21][C:14]([CH2:15][NH:16][CH2:17][CH2:18][O:19][CH3:20])=[CH:13][CH:12]=1.C(N(CC)CC)C>ClCCl>[CH3:9][O:10][C:11]1[CH:22]=[CH:21][C:14]([CH2:15][N:16]([CH2:17][CH2:18][O:19][CH3:20])[C:5]([Cl:8])=[O:4])=[CH:13][CH:12]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 10426DiphosgeneHCID 32858732-methoxy-N-(4-methoxybenzyl)ethanamine

Produkt 1

HCID 219560334-Methoxybenzyl(2-methoxyethyl)carbamoyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

0.51 g (0.31 ml, 2.56 mmol) of trichloromethyl chloroformate (“diphosgene”) are dissolved in 15 ml of dichloromethane, and 1.00 g (5.12 mmol) of 4-methoxybenzyl(2-methoxyethyl)amine and 0.78 g (7.68 mmol) of triethylamine are slowly added. After stirring at room temperature overnight, the mixture is poured into ice-water and extracted three times with dichloromethane, and the organic phase is dried over magnesium sulfate and concentrated to dryness in a rotary evaporator. The crude product is employed without workup directly in the next stage.

Aufarbeitung

  1. extractionextracted three times with dichloromethane
  2. dry with materialthe organic phase is dried over magnesium sulfate
  3. concentrationconcentrated to dryness in a rotary evaporator

Quellen und Nachweise

ORD-Eintrag
ord-18912abb5e604afb8af2d2a4c934ad19
Quelldatensatz
uspto-grants-2006_09
Patentnummer
US07105523B2

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