تفاعل #1166462

معادلة التفاعل

3-methoxy-4-hydroxy-7-acetoxy-2H-l-benzopyran-2-one

benzyl bromide

sodium carbonate

→

title compound

المردود 37.0%

3-methoxy-4-benzyloxy-7-acetoxy-2H-1-benzopyran-2-one

المردود 37.0%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe solid in the reaction mixture was filtered off
2. 2
   workup.ADDITIONthe filtrate was poured into 200 ml of water
3. 3
   استخلاصextracted with 500 ml of benzene
4. 4
   تركيزThe organic layler was concentrated in vacuo
5. 5
   تجفيفafter drying over magnesium sulfate
6. 6
   أخرىto give oily residue
7. 7
   أخرىThe residue was purified on silica gel column chromatography (eluent: benzene/ethyl acetate=7/3)

الإجراء التجريبي

To a mixture of 8.11 g of 3-methoxy-4-hydroxy-7-acetoxy-2H-l-benzopyran-2-one (27.8 mmol) and 5.71 g of benzyl bromide (33.4mmol) in 50 ml of DMF was added 4.61 g of sodium carbonate (33.4 mmol) under argon atmosphere, then the mixture was stirred at 50° for 2 hours. The solid in the reaction mixture was filtered off, the filtrate was poured into 200 ml of water and extracted with 500 ml of benzene. The organic layler was concentrated in vacuo after drying over magnesium sulfate to give oily residue. The residue was purified on silica gel column chromatography (eluent: benzene/ethyl acetate=7/3) to give 3.50 g of the title compound. (yield=33%)

المصدر