Acetic Anhydride → N-[2-(tert-Butoxycarbonylmethylamino)ethyl]-N-methylacetamide

HRID 17494Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 17494
C(OC(=O)C)(=[O:3])C.[CH2:8]([N:10]([CH2:13][CH3:14])[CH2:11][CH3:12])C.[C:15]([O:19][C:20]([CH2:22][NH:23]CCNC)=[O:21])([CH3:18])([CH3:17])[CH3:16]>ClCCl>[C:15]([O:19][C:20]([CH2:22][NH:23][CH2:12][CH2:11][N:10]([CH3:8])[C:13](=[O:3])[CH3:14])=[O:21])([CH3:18])([CH3:17])[CH3:16]

Komponenten

5

Edukt 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 59921864HCID 59921864, Verbindung

Produkt 1

HCID 86630858N-[2-(tert-Butoxycarbonylmethylamino)ethyl]-N-methylacetamideAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Under nitrogen atmosphere, acetic anhydride (1.16 ml, 12.3 mmol) and triethylamine (2.28 ml, 16.4 mmol) were added to a dichloromethane (41 ml) solution of [2-(tert-butoxycarbonylmethylamino)ethyl]methylamine (I-202) (1.54 g, 8.18 mmol) with cooling with ice, followed by stirring at room temperature for 15 hours. The solvent was evaporated away under reduced pressure, then the resulting residue was subjected to silica gel column chromatography, and the eluate with dichloromethane/methanol (10:1, v/v) gave the entitled compound (1.88 g, 100%) as a colorless oil.

Aufarbeitung

  1. temperaturewith cooling with ice
  2. customThe solvent was evaporated away under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-422600918c5448baa5b1af786fee5d8d
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07737166B2

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