Reaktion #997653

Reaktionsgleichung

ethanolamine

Perfluoro-2-methyl-3-oxahexanoyl fluoride

→

N-(perfluoro-2-methyl-3-oxahexanoyl)-2-aminoethanol

Lösungsmittel

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe reaction temperature below 25° C
2. 2
   workup.ADDITIONAfter the addition
3. 3
   SonstigeThe solid was removed by filtration
4. 4
   Waschenthe filtrate was washed with hydrochloric acid (0.5N, 30 mL), water (2 times 30 mL), sodium hydrogen carbonate solution (0.5N, 20 mL), water (30 mL), and sodium chloride solution (saturated, 20 mL)
5. 5
   EinengenIt was then concentrated
6. 6
   Sonstigedried in vacuum over night at room temperature

Vorschrift

A mixture of ethanolamine (13 g, 28 mmol) and ether (30 mL) was cooled to 15° C. Perfluoro-2-methyl-3-oxahexanoyl fluoride (33 g in ether 50 mL) was added dropwise to keep the reaction temperature below 25° C. After the addition, the reaction mixture was stirred at room temperature for one hour. The solid was removed by filtration and the filtrate was washed with hydrochloric acid (0.5N, 30 mL), water (2 times 30 mL), sodium hydrogen carbonate solution (0.5N, 20 mL), water (30 mL), and sodium chloride solution (saturated, 20 mL). It was then concentrated and dried in vacuum over night at room temperature to give N-(perfluoro-2-methyl-3-oxahexanoyl)-2-aminoethanol as a white solid 35 g, yield 95%. mp. 69-72° C. 1H NMR (CDCl3) δ 1.67 (bs, 1H), 3.57 (m, 2H), 3.80 (t, J=5 Hz, 2H), 6.91 (bs, 1H).

Quelle