反应详情

温度

180 °C

A stirred, homogeneous mixture of finely powdered, compound 27 (17.0 g, 0.10 mol), aluminium chloride (29.4 g, 0.22 mol) and sodium chloride (7.1 g, 0.12 mol) was heated to 180° C. over 25 min and then at 180° C. for 1 h (glc and tlc analyses both revealed a complete reaction). Ice-water was added, and the product was extracted into ether (twice). The combined ethereal extracts were washed with water, and the product was extracted into 10% sodium hydroxide (twice) and the combined basic extracts were acidified with 36% hydrochloric acid. The product was extracted into ether (twice), and the combined ethereal extracts were washed with water and dried (MgSO4). The solvent was removed in vacuo to give a fawn solid.

1. customa complete reaction)
2. extractionthe product was extracted into ether (twice)
3. washThe combined ethereal extracts were washed with water
4. extractionthe product was extracted into 10% sodium hydroxide (twice) and the combined basic extracts
5. extractionThe product was extracted into ether (twice), and the combined ethereal extracts
6. washwere washed with water
7. dry with materialdried (MgSO4)
8. customThe solvent was removed in vacuo
9. customto give a fawn solid