Hydrochloric Acid → HCID 20135775, compound

Temperature

70 °C

A mixture consisting of 6 g of the 3-amino-5,7-dinitroindazole, 18 g of iron powder, 60 ml of methyl alcohol, 30 ml of water and 3 ml of hydrochloric acid was stirred for 1.5 hours at 70° C. After cooling the reaction mixture, the mixture was filtered. The pH of the filtrate was adjusted to 11 with a potassium carbonate solution, and the filtrate was extracted three times with 50 ml of ethyl acetate. The ethyl acetate layer was washed with water and dried over anhydrous sodium sulfate, and ethyl acetate was removed under reduced pressure. The residue thus obtained was subjected to an alumina-column chromatography(alumina: 200 g) using chloroform as the developing solvent to give 0.85 g of 3,5,7-triaminoindazole having the following analytical values in a yield of 19%.

1. temperatureAfter cooling the reaction mixture
2. filtrationthe mixture was filtered
3. extractionthe filtrate was extracted three times with 50 ml of ethyl acetate
4. washThe ethyl acetate layer was washed with water
5. dry with materialdried over anhydrous sodium sulfate, and ethyl acetate
6. customwas removed under reduced pressure
7. customThe residue thus obtained

ORD record

ord-94db3519c3064e7da1ffb3e1d8377641

Source dataset

uspto-grants-1985_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04533731