반응 #1552056

반응 방정식

5-allyloxy-2-nitrobenzyl alcohol

m-chloroperoxybenzoic acid

→

5-glycidyloxy-2-nitrobenzyl alcohol

용매

dichloromethane

반응 조건

후처리

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

실험 절차

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.

출처