Reaktion #452713

Reaktionsgleichung

Sodium borohydride

3-bromo-4-methylaniline

acetic acid

acetone

sodium acetate

→

(3-Bromo-4-methyl-phenyl)-isopropyl-amine

Lösungsmittel

water

ethanol

hexane

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe layers were separated
2. 2
   Extraktionaqueous layer was extracted with ether/hexane (1:1)
3. 3
   WaschenThe combined organic layers were washed once with water and brine
4. 4
   Trocknendried with MgSO4
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated under reduced pressure
7. 7
   SonstigeThe residue was used directly for the next reaction without further purification

Vorschrift

Sodium borohydride (30.5 g, 806.2 mmol) was added slowly over 3 hours to a stirring mixture of 3-bromo-4-methylaniline (30 g, 161.2 mmol), ethanol (110 mL), acetic acid (92 mL, 1.6 mol), water (265 mL), acetone (66 mL, 892.2 mmol), and sodium acetate (29.2 g, 214.9 mmol). The solution was stirred at 0° C. for 1 hour. The reaction mixture was poured into the 1:1 mixture of ether and hexane containing 2N KOH. The layers were separated and aqueous layer was extracted with ether/hexane (1:1). The combined organic layers were washed once with water and brine, dried with MgSO4, filtered, and concentrated under reduced pressure. The residue was used directly for the next reaction without further purification:

Quelle