تفاعل #725879
ord-76c065a61fa446699c471066dc98e928
معادلة التفاعل
methyl salicylate
K2CO3
methyl chloroacetate
→
1
المردود 17.0%
2-Methoxycarbonylmethoxy-benzoic acid methyl ester
المردود 17.0%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةrefluxed for 36 hours
- 2workup.DISTILLATIONThe acetone was distilled off
- 3workup.ADDITIONwater (1200 ml) was added
- 4استخلاصCrude 1 was extracted into chloroform
- 5تجفيفdried over Na2SO4
- 6workup.DISTILLATIONdistilled
- 7أخرىpurified by column chromatography on silica gel
الإجراء التجريبي
To a mixture of methyl salicylate (100 g, 657 mmol) and anhydrous K2CO3 (360 g, 2.605 mol) in anhydrous acetone (1000 ml) was added methyl chloroacetate (94 g, 866 mmol) and refluxed for 36 hours. The acetone was distilled off and water (1200 ml) was added. Crude 1 was extracted into chloroform, dried over Na2SO4 distilled and purified by column chromatography on silica gel using hexane as eluant to give pure 1 (25 grams, 17%) as a light yellow syrup.