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Toluene → HCID 59370775, Verbindung

HRID 1678722
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1678722
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([O:11][Si:12]([CH2:17][CH3:18])([CH2:15][CH3:16])[CH2:13][CH3:14])[CH2:9]I)=[CH:4][C:3]=1[NH:19][S:20]([CH3:23])(=[O:22])=[O:21].[CH2:24]([NH:31][CH2:32][CH2:33][OH:34])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C1(C)C=CC=CC=1>CCOCC>[CH2:24]([N:31]([CH2:32][CH2:33][OH:34])[CH2:9][C@@H:8]([C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([NH:19][S:20]([CH3:23])(=[O:22])=[O:21])[CH:4]=1)[O:11][Si:12]([CH2:17][CH3:18])([CH2:15][CH3:16])[CH2:13][CH3:14])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1140TolueneHCID 4348BenzylethanolamineHCID 53922285HCID 53922285, Verbindung

Produkt 1

HCID 59370775HCID 59370775, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

(R)-N-(2-chloro-5-(2-iodo-1-(triethylsilyloxy)ethyl)phenyl)methanesulfonamide (3 g) and 2-(benzylamino)ethanol (6 mL; manufactured by Tokyo Chemical Industry Co., Ltd.) were mixed, and the mixture was stirred overnight at 100° C. The reaction solution was cooled to room temperature, and then toluene and Et2O were added thereto. The mixture was washed three times with water, and the organic layer was dried over magnesium sulfate. Then, the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=84:16→64:36), and thus the title compound (2.1894 g) was obtained.

Aufarbeitung

  1. temperatureThe reaction solution was cooled to room temperature
  2. washThe mixture was washed three times with water
  3. dry with materialthe organic layer was dried over magnesium sulfate
  4. customThen, the solvent was evaporated under reduced pressure
  5. customThe residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=84:16→64:36)

Quellen und Nachweise

ORD-Eintrag
ord-202e718141cf426db488aea094d95910
Quelldatensatz
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08008506B2

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