반응 #1355842

반응 방정식

methylene chloride

3-Bromo-1-propanol

5-hydroxy-2-nitrobenzaldehyde

K2CO3

→

desired product

수율 96.0%

2-Nitro-5-(3-hydroxypropoxy)benzaldehyde

수율 96.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   여과The mixture was filtered
2. 2
   세척the solid residue was washed with methylene chloride
3. 3
   기타The combined organic solution was evaporated to dryness
4. 4
   workup.DISSOLUTIONredissolved in 100 ml methylene chloride
5. 5
   세척The resulted solution was washed with saturated NaCl solution
6. 6
   건조dried over sodium sulfate

실험 절차

3-Bromo-1-propanol (3.34 g, 24 mmol) was refluxed in 80 ml of anhydrous acetonitrile with 5-hydroxy-2-nitrobenzaldehyde (3.34 g, 20 mmol), K2CO3 (3.5 g), and KI (100 mg) overnight (15 h). The reaction mixture was cooled to room temperature and 150 ml of methylene chloride was added. The mixture was filtered and the solid residue was washed with methylene chloride. The combined organic solution was evaporated to dryness and redissolved in 100 ml methylene chloride. The resulted solution was washed with saturated NaCl solution and dried over sodium sulfate. 4.31 g (96%) of desired product was obtained after removal of the solvent in vacuo.

출처