反应详情

To a solution of the compound obtained in Step C (47.48 mmoles) in acetonitrile (260 ml) there are added 1-bromomethyl-4-nitro-benzene (52.23 mmoles) and potassium carbonate (189.92 mmoles). The reaction mixture is stirred at reflux for 4 hours under nitrogen. The reaction mixture is brought to ambient temperature and then diluted with 500 ml of DCM and 100 ml of water. Extraction with DCM (2×200 ml) is carried out and then the organic phases are combined. The organic phase obtained is washed with saturated NaCl solution and is then dried over sodium sulphate, filtered and concentrated to about 75 ml. After formation of a precipitate in suspension, ethyl ether (150 ml) is added, and stirred is carried out overnight at ambient temperature. The precipitate is filtered off, washed with ethyl ether and dried in vacuo to yield the title product, which is used directly in the next Step.

1. temperatureat reflux for 4 hours under nitrogen
2. customis brought to ambient temperature
3. extractionExtraction with DCM (2×200 ml)
4. customThe organic phase obtained
5. washis washed with saturated NaCl solution
6. dry with materialis then dried over sodium sulphate
7. filtrationfiltered
8. concentrationconcentrated to about 75 ml
9. additionAfter formation of a precipitate in suspension, ethyl ether (150 ml) is added
10. stirringstirred
11. filtrationThe precipitate is filtered off
12. washwashed with ethyl ether
13. customdried in vacuo