Trifluoroacetic acid → 2-[2-(6-Chlorohexyloxy)ethoxy]ethylammonium trifluoroacetate

HRID 1397968Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1397968
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][NH:14]C(=O)OC(C)(C)C.[F:22][C:23]([F:28])([F:27])[C:24]([OH:26])=[O:25].ClCCl.CO>ClCCl>[F:22][C:23]([F:28])([F:27])[C:24]([O-:26])=[O:25].[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][NH3+:14]

Komponenten

5

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Under argon atmosphere, to a solution of tert-butyl N-[2-{2-(6-chlorohexyloxy)ethoxy}ethyl]carbamate (11) (synthesized by the method described in Non-Patent Document Y. Zhang, M.-k. So, A. M. Loening, H. Yao, S. S. Gambhir, J. Rao, Angew. Chem. Int. Ed., 2006, 118, 4936-4940) (84.2 mg, 260 pump in dichloromethane (2.5 mL) was added trifluoroacetic acid (0.5 mL) at 0° C. After stirring for 2 hours at the same temperature of 0° C., the starting compound 11 completely disappeared as judged from TLC study (Rf=0.41, dichloromethane/methanol=9/1). The reaction solution was then concentrated under reduced pressure using an evaporator to give crude 2-[2-(6-chloro hexyloxy)ethoxy]ethylammonium trifluoroacetate (12) as a colorless oil. The crude product was used in the next reaction without further purification.

Aufarbeitung

  1. concentrationThe reaction solution was then concentrated under reduced pressure
  2. customan evaporator

Quellen und Nachweise

ORD-Eintrag
ord-5ded7405e92c4027b150a23d4a9306c5
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08901312B2

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