تفاعل #1177
ord-33cc46ae4b86423a92b024e4bd6cb9eb
معادلة التفاعل
sodium
isopropyl ether
2,6-dimethoxyacetophenone
ethyl oxalate
sodium methylate
→
expected product
Methyl 4-(2,6-dimethoxyphenyl)-4-oxido-2-oxo-3-butenoate sodium salt
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةThe reaction mixture is heated
- 2درجة الحرارةto reflux for 7 hours
- 3workup.WAITleft
الإجراء التجريبي
A solution of 100 g of 2,6-dimethoxyacetophenone and 7.5 ml of ethyl oxalate in 520 ml of anhydrous MeOH is added slowly to a solution of sodium methylate prepared from 12.7 g of sodium and 285 ml of anhydrous MeOH. The reaction mixture is heated to reflux for 7 hours and left overnight at RT. It is poured into 2 litres of isopropyl ether and left stirring for 15 minutes. The expected product is obtained by filtration, washing with isopropyl ether and drying under vacuum, m=120 g, m.p.=178° C.