Hydrazine → HCID 21515433, compound

7 g. of 3-chloro-5-aminopyridazine is added to 125 ml. of hydrazine and the mixture is stirred under nitrogen for 17.5 hours at a temperature below reflux. The reaction mixture is cooled to room temperature, and the residual hydrazine removed by evaporation. The residue is treated with 250 ml. of methanol to extract the product. After separating the extractant and washing the residue with small amounts of methanol, the combined extractant-filtrate is treated with hydrogen chloride gas. The solution is then treated with ether to give a crystalline product which is recrystallized from methanol to give 5-amino-3-hydrazinopyridazine dihydrochloride; m.p. 220°-222°C.

1. temperaturebelow reflux
2. customthe residual hydrazine removed by evaporation
3. additionThe residue is treated with 250 ml
4. extractionof methanol to extract the product
5. customAfter separating the extractant
6. washwashing the residue with small amounts of methanol
7. additionthe combined extractant-filtrate is treated with hydrogen chloride gas
8. additionThe solution is then treated with ether
9. customto give a crystalline product which
10. customis recrystallized from methanol

ORD record

ord-e230a57f9374441daf7af5200a81fe3b

Source dataset

uspto-grants-1976_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03978057