反应详情

A mixture of 0.04 g (0.11 mmol) of 3-(4′-acetyl-biphenyl-4-yl)-N-(4-chloro-phenyl) -acrylamidine, 0.028 g (0.33 mmol) of methoxylamine hydrochloride and 0.027 g (0.33 mmol) of sodium acetate in 3 mL of methanol was heated under microwave (100 W, 5 min). Diluted with 20 mL of NaHCO3, it was extracted with two 10 mL portions of ethyl acetate. The combined organic extracts were washed with 10 mL of brine, dried over Na2SO4, filtered and concentrated. The residue was purified by preparative TLC eluting with 70% ethyl acetate in hexanes plus 1% NH4OH to give 0.004 g of N-(4-chloro-phenyl)-3-[4′-(1-methoxyimino-ethyl)-biphenyl-4-yl]-acrylamidine.

1. temperaturewas heated under microwave (100 W, 5 min)
2. extractionwas extracted with two 10 mL portions of ethyl acetate
3. washThe combined organic extracts were washed with 10 mL of brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by preparative TLC
8. washeluting with 70% ethyl acetate in hexanes plus 1% NH4OH