تفاعل #1355842

معادلة التفاعل

methylene chloride

3-Bromo-1-propanol

5-hydroxy-2-nitrobenzaldehyde

K2CO3

→

desired product

المردود 96.0%

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

المردود 96.0%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe mixture was filtered
2. 2
   غسيلthe solid residue was washed with methylene chloride
3. 3
   أخرىThe combined organic solution was evaporated to dryness
4. 4
   workup.DISSOLUTIONredissolved in 100 ml methylene chloride
5. 5
   غسيلThe resulted solution was washed with saturated NaCl solution
6. 6
   تجفيفdried over sodium sulfate

الإجراء التجريبي

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.

المصدر