تفاعل #2546

معادلة التفاعل

4-Chloromethyl-N-(2-methoxyphenyl)benzamide

calcium carbonate

dioxane water

→

title compound

المردود 88.3%

4-Hydroxymethyl-N-(2-methoxyphenyl)benzamide

المردود 88.3%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةof heating
2. 2
   درجة الحرارةunder reflux
3. 3
   ترشيحfiltering off the formed insoluble materials
4. 4
   أخرىthe organic solvent was removed by evaporation
5. 5
   استخلاصThe thus obtained residue was extracted with ethyl acetate
6. 6
   غسيلthe resulting organic layer was washed with saturated brine
7. 7
   تجفيفdried on anhydrous magnesium sulfate
8. 8
   أخرىAfter removing the solvent
9. 9
   أخرىby evaporation
10. 10
    أخرىthe resulting colorless solid material was purified

الإجراء التجريبي

4-Chloromethyl-N-(2-methoxyphenyl)benzamide (500 mg, 1.81 mmol) and precipitated calcium carbonate (970 mg, 9.7 mmol) were suspended in a dioxane-water (1:1) mixture solution (9 ml) and subjected to 25 hours of heating under reflux. After adding THF (25 ml) and filtering off the formed insoluble materials, the organic solvent was removed by evaporation. The thus obtained residue was extracted with ethyl acetate, and the resulting organic layer was washed with saturated brine and dried on anhydrous magnesium sulfate. After removing the solvent by evaporation, the resulting colorless solid material was purified by subjecting it to a silica gel column chromatography (ether:hexane=3:1), thereby obtaining 411 mg (88.3%) of the title compound in the form of colorless crystals.

المصدر