反应详情

6-Methoxy-4-[(5-nitro-2-thienyl)sulfanyl]-7-quinolinol (500 mg), 3-diethylaminopropanol (290 mg), diethyl azodicarboxylate (390 mg), triphenylphosphine (590 mg), tetrahydrofuran (30 ml), 1-methyl-2-pyrrolidinone (2 ml) and dimethylsulfoxide (10 ml) were stirred together at 0° C. for 5 hours and then at room temperature for 10 hours. Water was added, extraction was performed with ethyl acetate, and the extract was back extracted with 2N aqueous hydrochloric acid. After adding 5N aqueous sodium hydroxide to the hydrochloric acid extract and performing extraction with ethyl acetate, the extract was washed with water and then with saline and dried over magnesium sulfate. NH type silica gel was coated onto a glass filter, the ethyl acetate layer was passed through the filter, and the solvent was distilled off under reduced pressure to obtain 500 mg of a reddish-brown oil.

1. extractionextraction
2. extractionthe extract was back extracted with 2N aqueous hydrochloric acid
3. additionAfter adding 5N aqueous sodium hydroxide to the hydrochloric acid
4. extractionextract
5. extractionextraction with ethyl acetate
6. washthe extract was washed with water
7. dry with materialwith saline and dried over magnesium sulfate
8. filtrationfilter
9. distillationthe solvent was distilled off under reduced pressure