Reaktion #1552056

Reaktionsgleichung

5-allyloxy-2-nitrobenzyl alcohol

m-chloroperoxybenzoic acid

→

5-glycidyloxy-2-nitrobenzyl alcohol

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigepeaks disappeared from the 1H-NMR spectrum (approximately 48 hours)
2. 2
   WaschenThe reaction was then washed with aqueous sodium carbonate twice
3. 3
   Trocknenwater three times and then dried over sodium sulfate
4. 4
   SonstigeThe solvent was partially removed by rotary evaporation
5. 5
   workup.ADDITIONpoured into hexanes
6. 6
   Sonstigeto precipitate the product
7. 7
   FiltrationThe resulting solid was collected by suction filtration
8. 8
   Sonstigewas used in the next step without further purification

Vorschrift

5-allyloxy-2-nitrobenzyl alcohol (7.3 g, 35 mmol) and m-chloroperoxybenzoic acid (77 wt. %, 9.4 g, 42 mmol) were dissolved in dichloromethane and refluxed until the allyl peaks disappeared from the 1H-NMR spectrum (approximately 48 hours). The reaction was then washed with aqueous sodium carbonate twice, water three times and then dried over sodium sulfate. The solvent was partially removed by rotary evaporation and then poured into hexanes to precipitate the product. The resulting solid was collected by suction filtration and was used in the next step without further purification.

Quelle