Reaktion #66110

Reaktionsgleichung

Benzyl bromide

2-chloro-5-nitro-phenol

potassium carbonate

→

2-benzyloxy-1-chloro-4-nitro-benzene

Ausbeute 99.0%

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturat reflux for 2 h
3. 3
   FiltrationInorganic salts were filtered off
4. 4
   Waschenwashed with acetone (20 mL)
5. 5
   EinengenThe combined filtrate and washings were concentrated in vacuo
6. 6
   workup.DISSOLUTIONthe resulting residue then being dissolved in ethyl acetate (25 mL)
7. 7
   Waschenwashed successively with water (2×20 mL), brine (20 mL)
8. 8
   Trocknendried over anhydrous sodium sulfate
9. 9
   Einengenconcentrated in vacuo

Vorschrift

Benzyl bromide (0.6 mL, 5.04 mmol) was added dropwise to a mixture of 2-chloro-5-nitro-phenol (800 mg, 4.61 mmol) and potassium carbonate (1.27 g, 9.22 mmol) in acetone (20 mL) at room temperature and heated at reflux for 2 h. Inorganic salts were filtered off and washed with acetone (20 mL). The combined filtrate and washings were concentrated in vacuo, the resulting residue then being dissolved in ethyl acetate (25 mL) and washed successively with water (2×20 mL), brine (20 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to yield 2-benzyloxy-1-chloro-4-nitro-benzene (1.20 g, 99%) as a cream solid.

Quelle