反应详情

To 70 ml of ethyl alcohol was added 3.50 g of the 1-(3-diethylaminopropyl)-3-phthalimido-4-chloroindazole. The mixture was added with 85 % hydrazine hydrate under cooling with ice and stirred for 3 hours under cooling with ice. The reaction mixture was filtered and the filtrate was removed under reduced pressure. The residue thus obtained was added with 20 ml of water and extracted with chloroform. The chloroform layer was extracted with 2N hydrochloric acid. The pH of the hydrochloric acid layer was adjusted to 10 with potassium carbonate, and the alkali layer was extracted with chloroform. The chloroform layer was dried over anhydrous sodium sulfate and filtered. The filtrate was removed under reduced pressure to give 2.03 g of 1-(3-diethylaminopropyl)-3-amino-4-chloroindazole having the following analytical values in a yield of 85 %.

1. temperatureunder cooling with ice
2. temperatureunder cooling with ice
3. filtrationThe reaction mixture was filtered
4. customthe filtrate was removed under reduced pressure
5. customThe residue thus obtained
6. extractionextracted with chloroform
7. extractionThe chloroform layer was extracted with 2N hydrochloric acid
8. extractionthe alkali layer was extracted with chloroform
9. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
10. filtrationfiltered
11. customThe filtrate was removed under reduced pressure