Reaktion #598891

Reaktionsgleichung

3,5-dinitrobenzoic acid

sodium hydrogen carbonate

sodium iodide

6-chlorohexanol

→

6-hydroxyhexyl 3,5-dinitrobenzoate

Ausbeute 91.0%

Lösungsmittel

1-methyl-2-pyrrolidone

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture is heated up to 90° C
2. 2
   Temperaturis heated to 100° C. for 1 h
3. 3
   SonstigeAfter 1 h of reaction
4. 4
   FiltrationThe product is filtrated
5. 5
   Waschenwashed water
6. 6
   Sonstigedried at 50° C. under vacuum for 24 h

Vorschrift

357.70 g (1.686 Mol) of 3,5-dinitrobenzoic acid is suspended in 750 ml of 1-methyl-2-pyrrolidone. The suspension is stirred up to 50° C. 386.36 g (4.599 Mol) of sodium hydrogen carbonate are added and the mixture is heated up to 90° C. 22.50 g (0.150 Mol) of sodium iodide and 204.0 ml (1.533 Mol) of 6-chlorohexanol are added to the reaction mixture which is heated to 100° C. for 1 h. After 1 h of reaction, the reaction is complete and the orange suspension is thrown on 2 l of ice and 1 l of water. The product is filtrated, washed water and dried at 50° C. under vacuum for 24 h to give 425.0 g (91%) of 6-hydroxyhexyl 3,5-dinitrobenzoate as a rose powder.

Quelle