反応 #1355842

反応方程式

methylene chloride

3-Bromo-1-propanol

5-hydroxy-2-nitrobenzaldehyde

K2CO3

→

desired product

収率 96.0%

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

収率 96.0%

溶媒

acetonitrile

反応条件

後処理

1. 1
   ろ過The mixture was filtered
2. 2
   洗浄the solid residue was washed with methylene chloride
3. 3
   その他The combined organic solution was evaporated to dryness
4. 4
   workup.DISSOLUTIONredissolved in 100 ml methylene chloride
5. 5
   洗浄The resulted solution was washed with saturated NaCl solution
6. 6
   乾燥dried over sodium sulfate

実験手順

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.

出典