反应详情

A mixture of 6 g (31 mmoles) of the compound obtained in Example 4, 6 mL (61 mmoles) of 1-bromo-3-chloropropane, 4.3 g (31 mmoles) of anhydrous potassium carbonate in 100 mL of acetone and 25 mL of N,N-dimethylformamide was heated at reflux for 16 hours. The reaction mixture was poured onto 100 mL of water and extracted with 100 mL of ethyl acetate. The organic extracts were washed with two portions of 100 mL of water, dried over sodium sulphate and evaporated at vaccum. The residue obtained was suspended in 25 mL of ethyl ether, filtered and dried at vaccum to give 4.2 g of 7-(3-chloropropoxy)-2-(hydroxymethyl)-chromen-4-one in 50% yield, mp 110-112° C.

1. temperaturewas heated
2. temperatureat reflux for 16 hours
3. extractionextracted with 100 mL of ethyl acetate
4. washThe organic extracts were washed with two portions of 100 mL of water
5. dry with materialdried over sodium sulphate
6. customevaporated at vaccum
7. customThe residue obtained
8. filtrationfiltered
9. customdried at vaccum