Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | 1-((2-Fluorophenyl)methyl)-1H-pyrazolo(3,4-b)pyridine-3-carboximidamide hydrochloride | HCID 57415844 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178512735 | HCID 178512735 | — |
Reaction Steps
50.000 g (163.535 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboximidamide hydrochloride were dissolved in 700 ml of ethanol, and 66.192 g (654.141 mmol) of triethylamine and 10.233 g (163.535 mmol) of hydrazine hydrate (80% strength solution in water) were added at 0° C. The mixture was stirred at RT overnight and then concentrated on a rotary evaporator. The residue was taken up in ethyl acetate and the solution was washed three times with saturated aqueous sodium chloride solution. The organic phase was dried over sodium sulphate and concentrated on a rotary evaporator. The residue was stirred with diethyl ether, filtered off with suction and dried under high vacuum. 46.49 g (46% of theory, 68% pure) of the title compound were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09133191B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-bfb932f1374d445dbb475769fa7121e9 |
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| Source note | uspto-grants-2015_09 |
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