Reaktion #504136

Reaktionsgleichung

bromomethylmethyl ether

triethylamine

→

triethyl(methoxymethyl)ammonium bromide

Ausbeute 85.0%

Lösungsmittel

hexane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto react at 60 to 70° C. for 6 hours
2. 2
   workup.ADDITIONwas added for crystallization

Vorschrift

77 g (0.6 moles) of bromomethylmethyl ether (a reagent available from Tokyo Chemical Industry Co., Ltd.) was added dropwise in 51 g (0.5 moles) of triethylamine (a reagent available from Tokyo Chemical Industry Co., Ltd.), and the mixture was allowed to react at 60 to 70° C. for 6 hours. After completion of the reaction, hexane was added for crystallization, thereby obtaining 96 g (percent yield: 85%) of a crystal of triethyl(methoxymethyl)ammonium bromide. 52 g (0.18 moles) of lithium bis(trifluoromethylsulfonyl)imide (a reagent available from Kanto Chemical Co., Inc.) was added to 34 g (0.15 moles) of this triethyl(methoxymethyl)ammonium bromide, and the mixture was allowed to react in an aqueous system. Subsequently, the reaction mixture was stirred for aging at room temperature for 3 hours. After completion of stirring, a lower layer (product) was separated. The separated product was washed with pure water four times and then washed with hexane four times. After completion of washing, the product was dried in vacuo at 100° C. and at a degree of vacuum of 0.5 kPa for 5 hours. Confirmation of the thus obtained product was carried out by means of 1H-NMR, 13C-NMR and 19F-NMR. A yield of the product (colorless transparent liquid) was 59 g (percent yield: 93%)

Quelle